Document emaDRw9JDKM15bbrYayq9jv2E

p. 1 . ~Raa6_ 36gz INTERIM REPORT #23 Analysis of Sediment Samples STUDY TITL E Analysis of Perfluorooctanoic Acid (PFOA) in Water, Soil, Sediment, Fish, Clams, Vegetation, Small Mammal Liver and Small Mammal Serum Using LC/MS/MS for the 3M Decatur Monitoring Progra m DATA REQUIREMENTS EPA TSCA Good Laboratory Practice Standards 40 CFR 792 STUDY DIRECTOR Jaisimha Kesari P .E ., DEE Weston Solutions, inc . 1400 Weston Way West Chester, PA 19380 Phone : 610-701-376 1 INTERIM REPORT COMPLETION DATE May 2, 2006 PERFORMI NG LABORATORY Exygen Research 3058 Research Drive State College, PA 1680 1 Phone : 814-272-1039 STUDY SPONSOR 3M Company 3M Building 0236-01-B-10 St. Paul, MN 55144 Phone : 651-733-637 4 PROJECT Protocol Number : P0000760 Exygen Study Number. P0000760 Total Pages : 110 p. 2 Interim Report #23 - Analysis of Sediment Samples Exygen Study No. : P0000 760 GOOD LABORATORY PRACTICE COMPLIANCE STATEMENT Exygen Study Number P0000760, entitled "Analysis of Perfluorooctanoic Acid (PFOA) in Water, Soil, Sediment, Fish, Clams, Vegetation, Small Mammal Liver and Small Mammal Serum Using ;.CNS/MS for the 3M Decatur Monitoring Program," conducted for 3M Company, is being performed in compliance with EPA TSCA Good Laboratory Practice Standards 40 CFR 792 by Exygen Research, with one exception. The laboratory control an d control spikes for the direct injection and alternate SPE methods and the spiking procedures for the surrogate were not recorded promptly at the time of extraction. o hn Flaherty Principal Investigator Exygen Research 2--t Dat e Jaisimha Kesar' P.E., Study Director Weston Solutions, Inc . DEE 36__ Date LY Mic acl . antoro Date Sponso Representative 3M Co pany Exygen Research Page 2 of 110 p. 3 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 QUALITY ASSURANCE STATEMENT Exygen Research's Quality Assurance Unit reviewed Exygen Study Number P0000760, entitled, "Analysis of Perfluorooct anoic Acid (PFOA) in Water, Soil, Sediment, Fish, Clams, Vegetation, Small Mammal Liver and Small Mammal Serum Using LC/MS/MS for the 3M Decatur Monitoring Program" . All reviewed phases ' were inspected for conduct according to Exygen Research's Standard Operating Procedu res ; the Study Protocol, and all applicable Good Laboratory Practice Standards . All fi ndings were repo rted to the Exygen Principal Investigator and Management and to the Study Director . Phase Date Reported to Date Reported t o Date Principal Exygen Date Reported to Inspected Investigator Manattement Study Director 31 . Final Raw Data 5/2/06 Review and Interim Analytical Report Review 5/2/06 5/2/06 5/2/06 Lyd' afler Tec ical i4=d, Quality Ass ance Uni t ~Gb7 06 Date tNote : All . in-lab inspections will be documented in the QA statement for the final analytical report at the conclusion of the study . This QA statement involves only the review of the interim report and associated raw data. Exygen Research Page 3 of 110 p. 4 interim Report #23 - Analysis of Sediment Samples Exygen Study No . : POU00760 CERTIFICATION OF AUTHENTICITY This interim report, for Exygen Study Number P0000760, is a true and complete representation of the raw data. Submitted by : Exygen Research 3058 Research Drive State College, PA 16801 (814) 272-103 9 Principal Investigator, Exygen : 0. / /) ~ /AZ-O-Z I / Flaherty Vice President Exygen Researc h ~ Date Exygen Research Facility Management : AR Richard President Exygen R arch ni Date Study Direc r, Weston Solutions, Inc. ' DfO Jaisimha esari P .E ., DEE Dat Weston Solutions, Inc . Sponsor Representative, 3M Company: Uf~ Michael . S antoro Date Director f Regulatory Affairs Exygen Research Page 4 of l 10 ,-, p. 5 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 STUDY IDENTIFICATIO N Analysis of Perfluorooctanoic Acid (PFOA) in Water, Soil, Sediment, Fish, Clams, Vegetation, Small Mammal Liver and Small Mammal Serum Using LC/MS/MS for the 3M Decatur Monitoring Program PROTOCOL NUMBER: P0000760 EXYGEN STUDY NUIVIBER: P0000760 TYPE OF STUDY : Residue SAMPLE MATRIX : Sediment TEST SUBSTANCE : Perfluorooctanoic acid (PFOA) SPONSOR : 3M Company 3M Building 0236-01-B-10 St. Paul, MN 55144 STUDY DIRECTOR : Jaisimha Kesari P .E., DEE Weston Solutions, Inc . 1400 Weston Way West Chester, PA 19380 STUDY MONITOR : Michael A . Santoro 3M Company 3M Building 0236-01-B-10 St. Paul, MN 55144 PERFORMING LABORATORY : Exygen Research 3058 Research Drive State College, PA 1680 1 ANALYTICAL PHASE Study Initiation Date : 11/05/04 TIMETABLE : Interim Analytical Start Date : 04/27/06 Interim Analytical Termination Date: 04/30/06 Interim Report Completion Date : 05 102/06 Exygen Research Page 5 of 110 p. 6 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 PROJECT PERSONNEL The Study Director for this project is Jaisimha Kesari at Weston Solutions, Inc . The following personnel from Exygen Research were associated with various phases of this interim portion of the study : Name Title John Flaherty Vice President Karen Risha Scientist Paul Connolly Technical Lead-LC/MS Christine Edwards Technician Mark Ammerman Sample Custodia n Amy Sheehan Associate Scientist Brittany Kravets Technician Scott Crain Technician Frances Crespi Technician Devon Ingram Technician Christa Gallant Technician Exygen Research Page 6 of 110 p. 7 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 TABLE OF CONTENTS Page TITLE PAGE . ... .. . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . ... . . . . . . . . . . . .. . .. . . . . . . . . .. . .. . . . . . . . . . . .. . . . . . . . .. . . . . . . . . . . . . . .. . .. . . . . .. . . . .1 GOOD LABORATORY PRACTICE COMPLIANC .E STATEMENT . . . . . . . . . . . . . . . . . . .. . . . . . . . . ..2 QUALITY ASSURANCE STATEMENT . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . ..3 CERTIFICATION OF AUTHENTICITY . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4 STUDY IDENTIFICATION. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . .5 PROJECT PERSONNEL. . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . .. . . . . . . . . . .. . .. . . . . . . . . . . . . . . . . .. . .. . . . . . . . . . . . . . . . . . . . . .6 TABLE OF CONTENTS . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . .. . .. . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . .. . .. . . . . . . . . . . . . . . . . .. . . . 7 LIST OF TABLES . .--- . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . .8 LIST OF FIGURES . .. . . . . . . . . .. . . . . . . . . . .. . .. . .. . . . . . . . . . . .. . . . . .. . . . .. . . . .. . . . . . . . . . . . . .. . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . ... . . . .9 LIST OF APPENDICES . . ... . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . .. . . . .. . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . .. . . . . .. . . .10 1 .0 SUMMARY . . .. . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . .11 2 .0 OBJECTIVE . . . . . . . . . . . . . . . . . . .. . .. . . . . . . . . . . . . . . . . . . . . . . .. . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . .11 3 .0 INTRODUCTION . . . . . . . . . . . . . .. . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .12 4 .0 ANALYTICAL TEST SA .IVIPLES. . . . . . . . . . . . .. . . . . . . . . .. . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .-12 5 .0 REFERENCE MATERIAL . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . .12 6 .0 DESCRIPTION OF ANALYTICAL METHOD . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . .1 3 6 .1 Extraction Procedure For Sediment . .. . . . .. . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .13 6 .2 Direct Inject Extraction Procedure For Sediment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .14 6 .3 Additional SPE Extraction Procedure For Sediment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . .14 6 .4 Percent Solids Procedure For Sediment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .14 6 .5 P reparation of Standards and Fortification Solutions . . . . . . . . . . . . . . . . . . . . . . . . . . .. . .. . . . . . . . . . . . . . . . .14 6.6 Chromatography . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .16 6 .7 Instrument Sensitivity . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .16 6 .8 Description of LC/MS/MS Instrument and Operating Conditions . . . . . . . . . . . . . . . . . . . . . . . . . . .16 6 .9 Quantitation and Example Calculation . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . .. . . . . . . . . . . . . . . . . .. . . . . . . . ..1 7 7.0 EXPERIMENTAL DESIGN . . . . . .. . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . .. . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .19 8.0 RESULTS . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . .. . .. . . . . . .. . .. . . . . . . . . . . . . . . . . .. . .. . . . . . . . . . . . . . . . . .. . .. . . . . . .19 9 .0 CONCLUSIONS . . . . . . . .. . . . . . . .. . . . . . . . . . .. . . . . . . . . . . . .. . .. . . . . . .. . .. . . . . . . . . .. . . .. . . . . . . . . . . . . .. . . . . . . . .. . . . . . . . . . . .2 0 10 .0 RETENTION OF DATA AND SAMPLES . . . . . . . . . . . . . . . .. . .. . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2 0 Exygen Research Page 7 of 110 p. 8 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . :~ P000076 0 LIST OF TABLES PageTable I . Summary of PFOA in Sediment Samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . .. . . . . .. . . . . . . . . . . . . .22 Table H . Summary of PFOA in Direct Injection Sediment Samples .. . . .. . . . . . . . . . . . . . . .. . . . . . .23 Table III. Summary of PFOA in SPE Extracted Sediment Samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .24 Table W. Matrix Spike Recovery ofPFCA in Sediment Samples . . .. . .. . . . . . . . . . . . . . . . . . . . . . . . . . .25 Table V. Matrix Spike Recovery of PFOA in Direct Injection Sediment Samples . . . . . . .26 Table VI . Matrix Spike Recovery of PFOA in SPE Extracted Sediment Samples . . . . . . . . .27 Table VII . Surrogate Spike Recovery of 13C PFOA in Sediment Samples . . . . . . . . . . . . . . . . . . . . . .28 Table VIII. Surrogate Spike Recovery of 13C PFOA in Direct Injection Sedimen t Samples .. . . . . .. . . . .. . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . .29 Table IX. Surrogate Spike Recovery of13C PFOA in SPE Extracted Sediment Samples . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .: . . . . . . . . . . . . . . . . . . . . . . . . . .30 Table X . Total Percent Solids in Sediment Samples . . . . .. . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . .. . .31 Exygen Research Page 8 of 110 p. 9 Inte rim Report #23 - Analysis of Sediment Samples Exygen Study No. : P0000760 Figure 1 . LIST OF FIGURES Page Typical Calibration Curve for PFOA in Methanol . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .33 Figure 2 . Extracted Standards of PFOA in Methanol, 25 ng/L an d 50 ng/L, Respectively . . . , . . . . . .. . . . . . . . . . . . . . . . . . . , .. . . . . . . .. . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . .. . .. . .34 Figure 3 . PFOA in Reagent Blank, 0.4 ng/mL Fortified Reagent Spk A , and 4 .0 ng/mL Forti fi ed Reagent Spk B, Respectively. . . . .. . . . . . . . . . . . . . . . . . . . . . . .. . . . . .35 Figure 4 . Chromatogram Representing a Sediment Sample Analyzed for PFOA (Exygen ID : C0172392, Data Set : 042806D) .. . .. . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .3 6 Figure 5 . Typical Calibration Curve for 13C PFOA in Methanol . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . .. . .37 Figure 6 . Extracted Standards of'3C PFOA in Methanol, 25 ng(L and 50 n&/1' Respectively . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . .3 8 Figure 7 . 13C PFOA in Reagent Blank, 0 .4 ng/mL Forti fied Reagent Spk A, and 4 .0 ng/mL Fortified Reagent Spk B, Respectively. . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . .39 Figure 8 . Chromatogram Representing a Sediment Sample Analyzed fo r 13C PFOA (Exygen ID- C0172892, Data Set: 042806D) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .40 Exygen Research Page 9 of 110 P . 10 Interim Report #23 - Analysis of Sediment Samples Exygen Study No. : P0000760 LIST OF APPENDICES Pale Appendix A Study Protocol P0000760 (Exygen Study No . P0000760) with Analytical Method V0001782 : "Method of Analysis for the Determination of Perfluorooctanoic Acid (PFOA) in Sediment by LClMS/MS", and Protocol Amendments . . . . . . ... . .. . . . . . . . . . .. . . . . . . . . . . . . . . . . . . . . . .41 Exygen Research Page 10 of 110 P. 11 Interim Report #23 - Analysis of Sediment Samples Exygen Study No .: P0000760 1.0 SUMMARY Exygen Research extracted and analyzed sediment samples for the determination of perfluorooctan oic acid (PFOA) according to Exygen Method V0001782 (Appendix A) . The limit of quantitation for PFOA in sediment was 2.0 ng/g . The standard sediment method (V0001782) was o riginally used to extract all of the samples. Use of this method yielded poor spiking recoveri es for PFOA. Because of this, a direct injection method (Section 6.2) was used, which also yielded poor recoveries . Finally, an alternative SPE column extraction (Section 6.3) was used to analyze for PFOA and13C PFOA . Analytical results for th e analysis of PFOA in sediment samples extracted according to the method based on dry weight are summarized in Table I . Analytical results for the analysis of PFOA in sediment samples by direct injection, based on dry weight, are summarized in Table II . Analytical results for the analysis of PFOA in sediment samples by alternative SPE extraction, based on dry weight, are summarized in Table 111 . The overall average percent recovery standard deviation for PFOA in sediment samples based on wet weight was 73 16%. Fortification recoveries for the analysis of PFOA in sediment samples are summarized in Table IV . Fo rti fication recoveries for the analysis of PFOA in direct injec ti on sediment samples are summarized in Table V . Fortification recoveries for the analysis of PFOA in SPE extracted sediment samples are summarized in Table VI . The average percent recovery standard deviation for "C PFOA in sediment samples based on wet weight was 97 27%. Fort i fi cation recoveries for 13C PFOA in sediment samples based on wet weight are summarized in Table VII . Forti fication recove ries for 13C PFOA in direct injection sediment samples based on wet weight are summarized in Table VEIL Fortification recoveries for '3C PFOA in SPE extracted sediment samples based on wet weight are surnrnarized in Table IX . The total percent solids for sediment samples are detailed in Table X . 2.0 OBJECTIV E The objective of the analytical part of this study was to determine levels of perfluorooctanoic acid (PFOA) in sediment according to Protocol P0000760 ( Appendix A) . Exygen Research Page 11 of 110 p . 12 Interim Report #23 - Analysis of Sediment Samples Exygen Study No. : POOpp760 3.0 INTRODUCTION This report details the results of the analysis for the determination of PFOA in sediment using the analytical methods entitled, "V0001782 : Method of Analysis for the Determination of Perfluorooctanoic Acid (PFOA) in Sediment by LClMS/MS . " The study was initiated on November 05, 2004, when the study director signed protocol number P 0000760 . The analytical start date for this interim report was April 27, 2006 and the analytical termination date for this interim report was April 30, 2006 . 4.0 ANALYTICAL TEST SAMPLES Three sediment samples (Exygen ID : C0172892-C0172894) were received on wet ice on April 22, 2006 from Tim Frinak at Weston Solutions, Inc . The samples were logged in by Exygen personnel and placed in refrigerated storage. Sample login and chain of custody information is located in the raw data package associated with this interim report . Storage records will be kept at Exygen Research . 5.0 REFERENCE MATERIA L The analytical standard, PFOA, was purchased from Oakwood Products, Inc, and was received at Exygen on March 17, 2005 . The surrogate spiking standard, 13C labeled perfluorooctanoic acid (13C PFOA SPtX}04184), was received at Exygen on April 15, 2004 from the 3M Company . The available information for the reference materials is listed below. PFOA was stored ambient and13C PFOA was stored frozen . Compound Entten InventorvNo . Lot # hjdVj%j PFOA SP0005444 203 99 13C PFOA SP0004184 3507-195 97 Expiration Date 03/31/07 0 3/29109 The molecular structure of PFOA is given below, PFOA Chemical Name: Perfluorooctanoic acid Molecular Weight : 41 4 Transitions Monitored : 413 -a 369 (for quantification) and 413 -* 219 (for confirmation) Structure : Exygen Research Page 12 of 110 p . 13 Interim Report #23 - Analysis of Sediment Samples Exygen Study No. : P0000760 F F F O F F F F F F F F OH FFF F 13C P1FOA Chemical Name: 1,2-13C perfluorooctanoic acid Molecular Weight: 41 6 Transition Monitored : 415 -~ 370 Structure: O F F F F F F ~ C 13C~ ~OH FFFFFF F 6.0 DESCRIPTION OF ANALYTICAL METHO D The analytical method "VO001782 : Method of Analysis for the Determination of Perfluorooctanoic Acid (PFOA) in Sediment by LC/MS/MS" was used for the sediment samples in this study. 6.1 Extraction Procedure For Sediment Before the samples were weighed for the extraction, they were mixed thoroughly by vigorously shaking the container. A 5 gram portion of sediment was weighed into a fifty milliliter centrifuge tube for the extraction. After fortification of appropriate samples, 35 mL of 1% acetic acid in water was added to the samples. The samples were vortexed and allowed to shake on a wrist action shaker for -60 minutes . The samples were centrifuged for -20 minutes at -3000 rpm. The supernatant was then loaded onto a Cle SPE cartridge conditioned with 10 mL of methanol and 20 mL of water . The eluate was discarded. Twenty milliliters of methanol was added to the sediment samples left in the centrifuge tube . The samples were vortexed and allowed to shake on a wrist action shaker for another 30 minutes . The samples were centrifuged again for -20 minutes at -3000 rpm . The supernatant was then loaded onto the same C18 SPE cartridge . The eluate was collected into a 500 mL Nalgene Bottle. The column was washed with 4 mL, of methanol. The wash was collected in the same bottle as the eluate . Approximately two Exygen Research Page 13 of 110 p . 14 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 hundred milliliters of water was added to the bottles . The samples were mixed by shaking and loaded onto another Ci e SPE cartridge conditioned with 10 mL of methanol and 20 niL of water . The eluate was discarded. Approximately five milliliters of methanol was added to the cartridge . Five milliliters of eluate was collected into a graduated 15 mL polypropylene centrifuge tube . Each sample was analyzed by LC/MS/MS electrospray. 6 .2 Direct Inject Extraction Procedure For Sedimen t Before the samples were weighed for the extraction, they were mixed thoroughly by vigorously shaking the container. A one-gram portion of sediment was weighed into a 15-milliliter centrifuge tube for the extraction . Ten milliliters of 1% acetic acid in methanol was added to each sample . The samples were then shaken by hand, vortexed, and sonicated for thirty minutes . The samples were then centrifuged for - 10 minutes at - 3000 rpm . Each sample was analyzed by LC/MS/MS electrospray, 6.3 Additional SPE Extraction Procedure For Sedimen t The samples that were prepared in 1% acetic acid for the direct injection method were used for this extraction . Five milliliters of each sample was aliquoted into a 50-mL polypropylene centrifuge tube and the volume was taken to 40 mL with water . The samples were then centrifuged for - 10 minutes at - 3000 rpm. The supernatant was then loaded onto a C,R SPE cartridge conditioned with 10 mL of methanol and 5 mL of water . The eluate was discarded . Approximately five milliliters of methanol was added to the cartridge . Five milliliters of eluate was collected into a graduated 1 5 mL polypropylene centrifuge tube . Each sample was analyzed by LC/MS/MS ele,,^trospray . 6.4 Percent Solids Procedure For Sedimen t Percent solids were determined using the procedure indicated in Exygen method V0000427. Approximately 20 grams of sample was weighed into a pan. The weight of the sample plus the pan was recorded . The samples were then dried in an oven overnight at 104 t 2C. Then the samples were transferred to a dessicator and allowed to cool for -15 minutes. Each sample was then weighed again, including the weight of the pan . The percent solid for each sample was then calculated . See Table X for percent solids results . 6.5 Preparation of Standards and Fortification Solution s A mixed stock standard solution of PFOA and 13C PFOA was prepared at a concentration of 1000 g/mL by dissolving 100 mg of each of the standards (corrected for purity and Exygen Research Page 14 of I 10 p . 15 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P000076 0 salt content) in 100 nil. of methanol . From this solution, the following fortification standards were prepared : Conc . of Fort Final Final Conc . of Stock or Fort. Volume Volume Fortification Std . Solution (mL) (mL) (g(mL) iH&LM L) i 1000 10 100 100 100 10 100 10 10 10 100 1 .0 1 .0 10 100 0.1 0 .1 10 100 0 .01 of PFOA and13C PFOA A stock solution of only 13C PFOA was also prepared at a concentration of 100 g/ml., by dissolving 10 mg the standard (corrected for purity and salt content) in 100 mL of methanol . From this solution, the following fortification standards were prepared : Conc . of Fort Final Final Conc . of Stock or Fort. Volume Volume Fortification Std . Solution (mL) (mL) (g/ml-) ( g/mo l 100 10 1 .0 of 13C PFOA 10 100 10 100 10 100 10 1 .0 0 .1 A set of non-extracted calibration standards containing PFOA and 1 3C PFOA was prepared in methanol, as specified in Exygen method V0001782 . The following concentrations were prepared Conc. of Fort Fort Final Final Cone. of or Calibration Volume Volume Calibration Std . (Sn olu) , tion (mL) (mL) (nghnL) LM 100 1 .0 10 10 100 0.5 10 5 .0 100 0 .2 10 2.0 to 1 .0 10 1 .0 5 .0 1 .0 10 0 .5 2 .0 1 .0 10 0 .2 ' of PFOA and13C PFOA Exygen Research Page 15 of 110 p . 16 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 The standards at final concentrations of 10, 5 .0, 2 .0, 1 .0, 0 .5 and 0 .2 ng/mL were used for calibration. Extracted calibration standards were prepared following method V0001780 . The stock standard solution and all fortification and calibration standard solutions were stored in a refrigerator (4 2C) when not in use . Documentation of standard preparation is located in the raw data package associated with this interim report . 6.6 Chromatograph y Quantification of PFOA was accomplished by LC/MS/MS electrospray . The retention time of PFOA was ---11 .1 min . Peaks above the LOD were not detected in any of the reagent blank samples corresponding to the analyte retention time . 6 .7 Instrument Sensitivity The smallest standard amount injected during the chromatographic run had a concentration of 0.2 ng/mL of PFOA. 6 .8 Description of LC/MS/MS Instrument and Operating Conditions Instrument : API 4000 Biomolecular Mass Analyzer Interface : Turbo Ion Spray Liquid Introduction Interface Computer: DELL OptiPlex GX400 Software: Windows NT, Analyst 1 .4 . 1 HPLC : Hewlett Packard (HP) Series 1 ; 00 HP Quat Pum p HP Vacuum Degasser HP Autosainpler HP Column Oven HPLC Column : Thermo Fluophase RP, 50 mm x 2 .1 nun Column Temp . : ~30 C Injection Vol . : 15 L Mobile Phase (A) : 2 mM Ammonium Acetate in water Mobile Phase (B): Methano l Time (min) % A %S 0 .0 65 35 1 .0 65 35 8 .0 25 75 10 .0 25 75 11 .0 65 35 18 .0 65 3 5 Exygen Research Page 16 of 110 p . 17 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 Total run time : --18 min Flow Rate: 0 .3 mUsnin Ions monitored : Approximate Anal yte Mode Transition Retention Time Moitored blinj PFOA negative 413-+369 - 11 .1 min . PFOA Confirm Ion negative 413-+219 - 11 .1 min . 13C PFOA negative 415-+370 -r11 .1 min . 6.9 Quantitation and Example Calculatio n PFOA concentrations are quantitated in nanogram of PFOA per milliliter of extract and then converted to nanogram per gram. The PFOA concentrations were quantitated in nanogram of PFOA per liter for Set #3 (Set 042806D) . Fifteen microliters of sample or calibration standard were injected into the LC/MS/MS. The peak area was measured and the standard curve was generated (using 1/x fit weighted linear regression) by Analyst software using seven concentrations of standards . The concentration was determined from the equations below. Please note that the equations in this section are presented in a different order than the equations in the method (V0001782), but this has no effect on the final calculations . Equation I calculated the amount of analyte found (in ng/L .., based on peak area) using the standard curve (linear regression parameters) generated by the Analyst software program . Equ~tion 1- Analyte found (ng/L) _ (Peak area - intercept) x DF Slope Where: DF = Dilution Factor, factor by which the final volume was diluted, if necessary . For samples fortified with known amounts of PFOA and13C PFOA prior to extraction, Equation 2 was used to convert the amount of PFOA found in ng/L to ng(g (ppb) . Equation 2 : PFOA found (ppb) TPFOA found (n /g_LLx SPE volume extracted ] [sample aliquot volume x (sample weight / direct inject sample volume)) Exygen Research Page 17 of 110 p . 18 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P000076 0 Equation 3 was used to calculate the percent recovery . Equation 3 : Recovery (%) _ (analvte found (nz(g wet weiaht? - analyte in control (ngJg wet weight)) amount added (ng/g, wet weight ) x 100!0 Note : For the PFOA recovery calculation, the "contml" is the unspiked aliquot of the primary field sample . Equation 4 was then used to calculate the amount of PFOA found in ppb based on dry weight. E.,auation 4: PFOA found (ppb) dry weight = PFOA found (ppb) x [100% / total solids('/a)] An example of a calculation using an actual sample follows : Sediment sample Exygen ID C0172892 Spk D (Set : 042806D), fortified at 4 ng/mL with PFOA where : peak area = 236588 intercept = 4630 slope = 420 dilution factor = 100 ng/g PFOA added (fort level) = 4000 arnt in corresponding sample (nglg) 596 SPE volume extracted (L) = 0.04 sample aliquot volume (niL) = 5 sample weight (g) = 1 direct inject sample volume (mL) 10 total solids (%) = 66 .54 From equation 1 : Analyte found (ng/L) = L236588 - 46301 x 100 420 = 55200 ng/L From equation 3 : PFOA found (ppb) (55200 nglL x 0 .04 L) 15mLx(1g/10mL)] = 4420 pp b From equation 3 : % Recovery = (4420 ng,/g - 586 n W&) x 100% 4000 ng/g = 96% Exygen Research Page 18 of 110 P . 19 interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 From equation 4 : PFOA found (ppb) dry weight = 4416 ppb x(100l0 / 66 .54%) = 6640 ppb NOTE: This value may be slightly different than that of the raw data due to rounding . 7.0 EXPERIMENTAL DESIGN 13C PFOA was used as a surrogate for all the samples . t3C PFOA was added to the sediment samples in the laboratory after the samples were weighed for extraction . For sediment samples designated as laboratory matrix spikes, PFOA was also added at a known concentration to the samples in the laboratory after the samples were weighed for extraction . The sediment samples were extracted in one set . The set included one reagent blank and two reagent blanks fortified at known concentrations . The set contained three sediment samples. For each sample, two laboratory matrix spikes and a duplicate were extracted . 8.0 RESULTS Analytical results for the analysis of PFOA in sediment samples based on dry weight are summarized in Table I . Analytical results for the analysis of PFOA in sediment samples by direct injection, based on dry weight, are summarized in Table Ii . Analytical results for the analysis of PFOA in sediment samples by alternative SPE extraction, based on dry weight, are summarized in Table III . The overall average percent recovery standard deviation for PFOA in sediment samples based on wet weight was 73 16% . Fortification recoveries for the analysis of PFOA in sediment samples are summarized in Table IV . Fortification recoveries for the analysis of PFOA in direct injection sediment samples are summarized in Table V . Fortification recoveries for the analysis of PFOA in SPE extracted sediment samples are summarized in Table VI . The average percent recovery standard deviation for ' 3C PFOA in sediment samples based on wet weight was 97 t 27% . Fortification recoveries for13C PFOA in sediment samples based on wet weight are summarized in Table VII . Fortification mcoveries for 'jC PFOA in direct injection sediment samples based on wet 'weight are summarized in Table VIII. Fortification recoveries for 13C PFOA in SPE extracted sediment samples based on wet weight are summarized in Table IX . The total percent solids for sediment samples are detailed in Table X. Exygen Research Page 19 of 110 p . 20 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 9.0 CONCLUSION S The sediment samples were successfully extracted and analyzed for PFOA using an alternative SPE method, which yielded acceptable QC data . 10.0 RETENTION OF DATA AND SAMPLES All original paper data generated by Exygen Research that pertains to this interim report will be shipped to the study director. This does not include facility-specific raw data such as instrument or temperature logs . Exact copies of all raw data, as well as a signed copy of the interim analytical report and all original facility-specific raw data, will be retained in the Exygen Research archives for the period of time specified in EPA TSCA Good Laboratory Practice Standards 40 CFR 792 . Exygen Research Page 20 of 110 p . 21 Interi m Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 TABLE S Exygen Research Page 21 of 110 p . 22 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 Table I. Summary of PFOA in Sediment Sample s Exygm ID Analyte Found (ppb, n9fq) Dry Weight Assessed CYent CI! Acid PFOA Accuracy Sample ID Perfluorooctanoic Add (.I- y.) C0172892 DAL-SO-OPP014)4MO MR N R C0172892 Rep DALSD4BPP01-0- 0000' NR NR C0172843 DAL-SD-BPP02-0-0000 NR NR C0172893 Rep DAL-SD-BPP02-0-0000' NR N R Co172894 DALSD-BPP03 -0A000 NR NR C0172894 Rep DAL-SD-BPP03-o-0000' NR NR 'Laboratory Oupk0a NR = Not reported due to queiiy c ontrol result iakwas. Sea Table 11 for re-anaysis results. Exygen Research Pagc 22 of 110 p . 23 Interim Report #23 - Analysis of Sediment Samples Exygen Study No. : P0000760 Table II. Summary of PFOA in Direct Injection Sediment Samples Exygen ID Cqent Analyte Found (ppb , ny1g) D ry Weight Assessed CA Acid PFOA Accuracy Sample ID Perfluorooctanolc Acid (+1- %) C0172892 D/1L-Sd-BPP0140000 NR NR C0172882 Rep D141.-SD-BPP01-D-0000 NR NR C0172893 DAL-SD-BPP02-0-0000 NR NR C0172893 Rep DAL-SD-BPP02-0-0000 NR NR C0172894 DAL-SA-BPP03-0-0000 NR N R C&172894 Rep DAL-SO-BPP03-0-0000 NR NR 'Laboratory Dupicaoe NR - Not reported due to quality control result feilures. See Table III for ra-analyefs results . Exygen Research Page 23 of 110 p . 24 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 Table III . Summary of PFOA in SPE Extracted Sediment Samples Cunt E:ypen b Sia%g ID Analyb round (ppb . npfp ) D ry Weight CC Acid PFOA PN11u0roott#nole Acid Atsaad Accuracy (+!-'b) C0172892 DAL-8 D-BPP01-0-0000 881 30 C0172892 Rep DAL-SD-8PP01-0-0000 945 30 COMM DALSDBPP02-0-0000 927 30 C0172893 Rep DAL-SD-BPP02-0-0000, 8 23 30 C0172894 DALS"PP03-0-0000 2390 30 C0172894 Rep DALSD-BPP03-. 0 0000 2380 30 'labonbry CupYCats Exygen Research Page 24 of 110 p . 25 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 Table IV. Matrix Spike Recovery of PFOA in Sediment Sample s Amount Amt Found Sample Spiked in Sarnpb wet weight CO Acid PFOA Amount Recovered Recovery wet t 1%) DAL-BD-BPP014)-000 0 iCOtr2aaa sppc D. soo ppb Spike) DAL-SO-BPP01-40000 K "'+san SO E. aooo 400 NR NR ppu sNwN 4000 NR NR NR NR DALSD4BPP02-0-000 0 Sco17311a ap AI c . 4oo PPe spWt<y 400 NR NR NR DAL-SD-BPP02-0-0000 "72a03 Ept t+. 4e00 PPe Sp" 4000 NR NR NR DALSD4BPP03-4OOOQ f CO+>zMS 3ok J . 4011 ppb Spike) 400 NR NR NR DAL-SD-BPP03-0-000 0 (Ca17 a " eWt K, 4000 PpbsWtca) 4000 NR NR NR Average : NR Standard DavlMlon: NR 5ampe residue e:aceeds the splxhp level apnifxsntly (3r apkirq bve l); therstoro, an sceurate mcovery valu e cannot be calcWated . NR = Not reported due to aiaity cororol result faikxee. See TabM V for re-aroyaia resuRS. Note: Since this aumea ry table shows minded rewift, recovery values may vary sUyMly from the values in the raw data. Exygen Research Page 25 of 110 p . 26 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 Table V. Matrix Spike Recovery of PFOA in Direct Injection Sediment Samples Sarnple Deaacl G8 Add PFOA Amount Amt Found Amoun t Spiked in Sample Recovered Recovery tlon we: t wet we !6 DALSD4BPP01-0-000 0 (ow'rzaa to D, aoao ODb><Ww3 DAL-SD-BPP01-0-0000 tco17m2 apc E, roooo PPb 4000 NR NR NR sa+a) 40000 NR NR MR DAL-S"PP02-0-0000 (=new apk c, +oeo vpa apruj DAL-SD-8PP92-0-0000 (0172sas spK H . ADM ppb spua) 4000 40000 NR NR NR NR NR NR DAL-SDBPP03-0-000 0 KA17290430 .1 , 40o0ppospbl 4000 NR NR NR DAL-SD-BPP03-0-0000 too17204 8pr K. 4ooeo Pvb aWW 40000 NR NR NR Average : NR Standad Dsvlatioo : NR 'Sample mstdue erceeds the spkinp loyal signx~caMy ( 3x epikinp leve ); therohxe, an aocurats recovery value cannot be calculate d NR a W reppiled due to quality oontrol m sult laalurna . See Table VI for nyarWysb msu ts . Kate, Since this summary taws shows roynded rasuNs, raeow ry values may vary slightly from the vakns in the raw data. Exygen Research Page 26 of 110 p . 27 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 Table YI. Matrix Spike Recovery of PFOA in SPE Extracted Sediment SaFnples CO Acid PFOA Amount Amt Found Amount Safftlya Spiksd in S arc oe Reooverod Description n wet wet WOW Recovery OAL-60-ePP0140000 (CO1720611 so D, 4000 nyo Splice) DAL-SD-BVP01 -40000 fcoaYsna at* E, 40091 aft sya Of DAL-SD-BPP02-40000 (CO172~q spY 6 IOeo npp ipibS DAt.-SO-BPP0240000 lootrnpa0 N,roooonsqsWk.1 4000 588 4420 98 40000 586 25600 83 4000 504 3860 84 40000 504 25100 61 DAL-SD-BPP03-40000 tCS+rnaa apt r, aoor rWy spl W 4000 DAL-sD-sPP03-a000 0 tcal72196 apk K. 4000 rpro spyky 40000 1080 4140 7 7 1080 23200 55 Avanpo : 73 Standard Devieson : 1 6 Mot: Sinu We sunvnary table shows rounded sults . roeow ry valws may v ery slightly from ehe, vahm in the aw data. 'Exygen Research Page 27 of 110 p . 28 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 Table VII . Surrogate Spike Recovery of "C PFOA in Sediment Samples Exygen ID Sample Description ,,C-PFOA Amount Amount Spiked Recovered Recovery (ng/p) Wet Weight (g6) (11919 ) C0172892 DAL-SD-BPP01-0-0000 4 NR NR C0172892 Rep DAL-SD4BPP01-0-0000 4 NR NR C0172892 Spk C DAL-SDBPP01-0-0000 4 NR NR C0172892 Spk D DAL-SD-BpPD1-0-0000 400 NR NR C0172892 Spk E DAL-SD-BPP01-0-0000 4000 NR N R C0172893 DAL-SD-BPP02-0-0000 4 NR NR C0172893 Rep DAL-SD-BPP02-00000 4 "NR NR C0172893 Spk F PAL-SD-BPP02-0-0000 4 " N R NR C0172893 Spk G DAL,SD-BPP02-0-0000 400' NR NR C0172893 Spk H DAL-SD-BPP02-0-0000 4000 NR N R C0172894 DAL-SD-BPP03-0-0000 4 NR NR C0172894 Rep DALSD-BPP03-0-0000 4 NR NR C0172894 Spk I DAL-SD-BPP03-0-0000 4 NR NR C0172894 Spk J DAL-SD-BPP03-0-0000 400 NR NR C0172894 Spk K DAL-SD-BPP03-0-0000 4000 NR N R Average : NR Standard Deviation: NR NR = Not reported due to quality control result failures. See Table VIII for re-analysis results. Note : Skim this s urrrnary table shows rounded results, recovery values may vary slightly from the values in the raw data. Exygen Research Page 28 of 110 p . 29 Interim Report #23 - Analysis of Sediment Samples Fxygen Study No . : P000076 0 Table VIII . Surrogate Spike Recovery of "C PFOA In Direct Injection Sediment Samples Exygen !a Amount Sample Spiked Description (no/9) "C-PFOA Amount Recovered Wet weight (n wB ) Recove ry (%) C0172892 DAL-SD-BPP01-0-M 40 NR NR C0172892 Rep DAL-SD-BPP01-0-OD00 40 NR NR C0 1 72892 Spk C DAL-SD-BPP01-0-0000 40 NR NR C0172892 Spk D DAL-SD-BPP01 4 0000 4000 NR NR C0172892 Spit E DALS"151501 -Q0000 40000 NR N R C0172893 DALSD-BPP02-0-0000 40 NR NR C0172893 Rep DAL-SD-BPP02-0-0000 40 MR NR C0172893 Spk F DAL-SD-BPP02-0-0000 40 NR NR C0172893 Spit G DAL-SD-BPP02- 0-0000 4000 NR NR C0172893 Spit H DAL-SD-BPP02-0-0000 40000 NR N R C0172894 DA1..-SD-BPP03-0-0000 40 NR MR C0172894 Rep DAL-SD-BPP03-0-0000 40 NR NR CD172894 Spk I DAL-SD-BPP03-0-0000 40 NR NR C0172894 Spk J DAL-SD-BPP03-Q0000 4000 NR NR C0172894 Spk K DAL-SD-BPP03-0-0000 40000 NR MR Averaqr NR Standard O ovtatlon : N R NR = Not reported due to quality control reault failuro"s . See Table IX for re,anelysls resuRs. Note: Since this summery table shows rounded results, recovery values may vary slightly from the values In the raw data. Exygen Research page 29 of l 10 p . 30 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P000076 0 Table IX. Surrogate Spike Recovery of 13C PFOA in SPE Extracted Sediment Samples Ezyqat Srnpe D Daapn "aPFoA Amount AmcLwk Svk.d Recovered Row," (ny9) weewefp h 00 C0172892 DAL-SD-8PP01-0-0000 40 52.0 130 C0172092 Rep 0AL-SD-BPP'0100000 40 51 .0 128 C0172882 Spk D OALSD-BPP014-0000 4000 375 0 4 C0172892 8pk E D.. AL-SD- M B -0-0000 6 40000 ~g00' 9 C0172893 DALSD-BPP02-04000 40 47 .8 C0172893 Rep DAI .-SD-8PP02-00000 40 51 .8 C017203 Spk (3 DAL-SD-BPP02-0-0000 4000 COt72893SpkH DAL-SD-BPP02-o-0000 40000 25200 120 129 3300 ga 63 C01728134 DAL-S0-BPP0343 .0000 40 45.2 113 C0172804 Rep DAL-SD-BPP034)-0000 40 40.3 101 c0172894 Spk J DALSDBPP03-0-0000 4000 9060 77 C0172894 Spk K DAL-SD-9PP03-0-0000 40000 22100 5 5 Note. Sincs Ills summary table Wwwa rounded results. recovery values may very a1fpAYY bom the values In the raw data. Average: 97 SbnOard Owlatl em 27 Exygen Research Page 30 of 110 p . 31 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 Table X. Total Percent Solids in Sediment Sample s Exyqon Sample ID Description Total Solids (%) C0172892 DAL-SD-BPP01-0-0000 66.54 C0172893 DAL-SD-BPP02-0-0000 54.37 C0172894 DAL-SD-BPP03-0-0000 44,48 Exygen Research Page 31 of 110 p . 32 Interim Report #23 - Analysis of Sediment Samples Exygcn Study No . : P0000760 ~ FIGURE S Exygen Research Page 32 of 110 p . 33 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0400760 Figure 1 . Typical Calibration Curve for PFOA in Methanol N o42lUOD sod. SPE.NOI r fO^T'Une srR*yesien Cl /~twi~M~~YayxQ :a403M003Q'~O .D7pS) 42a6 4Aa Q 7.866 3at6 3 .4Mf 3 .2 46 3D 66 2sa 2Ar6 !~1 2A.! 2.u.6 2.Os0 ~ 1 9. 8 i .E.lS 1 .M6 1 .263 1 .0~6 en.a 0 .064 . 4AN1 2.Oe4 OA D -1 00 200 300 460 800 000 C . .-6atimf. Fopll. 700 900 9 00 1000 Exygen Research Page 33 of 110 p . 34 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P000076 0 Figure 2 . Extracted Standards of PFOA In Methanol, 25 ng/L and 50 ngll,, Respectivel y , XC1N2 90&1 -PFOA (Shr4td) ITlKKi $ m s -sr+RpN 20144 Now 84290CAwM Mr: 1OZMUrrtr /A~ly~h x1MKi~I RY: 1rT.1n11 11A1 1200 goo so o 400 200 1 .62,1 .70 3 .80 -4.93 i . .i.0. 8.43 -11 .60 0 1 2 3 4 6 D 7 g 9 10 11 12 13 14 15 ta 17 Tim~, mi n , riC0 42B002 PFQA (6tbnda 4 413AX3L00 sinu ranyls 9 0140 horn 042600Dwifl Aru ! 2G169 eounb Na iqAt2 .14w003 ey RT :11 .1 nin 11A6 2000 CA 1S00 1(m0 800 OAO 44 1 AAS 0.848A1.8.3 4 Im 021~ 1 2 3 4 6 6 7 9 p 10 Tlm. mi. 11 12 13 14 16 10 17 Exygen Research Page 34 of 110 p . 35 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 Figure 3 . PFOA in Reagent Blank, 0 .4 ng/mL Fortified Reagent Spk A, and 4 .0 ngimL Fortified Reagent Spk B, Respectively , MM ur( Co~ PfOA %ft*W+ie)4fiVls! 9awr-i++tpN)e/Kfbo+rM2WiQw W #est aet h w"d) 400 O .yy~ a o .eo, cc 0140 1.32 3-W J+.w 0 .47edo 7.01 10.07 '11 .Da '11M 1 13. 11 14.12 te .4o MAO 1 2 3 9 0 0 7 0 p p tim e , mie ~ Ror0o e1SpYA-PFOA(OC) 4i3.0l3EOAarnuwmDl e lOoi 4E trom 0476060A" Area : 30296 enunk Height 2 .97 *+OOQ ops AT : 111 .0 min 11 12 13 14 16 10 17 41 .00 2000 tow 0 t0 e0 ~ 2 .00 7,EL 111 .00 13]0 1 2 3 4 6 0 7 0 0 t0 11 12 13 14 15 10 17 Tim e , We , R o apset Spit 6-PiOA(CC)4131DA00 .0 amdramplr, 11 M45 h @ rw0e2806D .w1e Area : 250300 wwAC Weight 2A6* 004 cps AT : 11 .1 min 2 .0e4 11 OE 1 .0r1 00 10A 1 2 3 4 6 0 7 6 0 10 71 t2 19 t4 t9 10 t7 tlmt . min Exygen Research Page 35 of 110 p . 36 Interim Report #23 -Analysis of Sediment Samples Exygen Study No . : P0000760 Figure 4. Chromatogram Representing a Sediment Sample Analyzed for PFOA (Exygen ID: C0172892, Data Set: 042806D) , Coll 2p~2 PFOA lGrt+ovr) 4ft 0 M la aw -wwrpn 0 of A000 KlN6aMW Ana: 3clC2f oer~tr I~JYk 170 +10.7cps RT7t~ Mr 3000 11D6 2000 2000 2i00 2200 2000 V 1800 CL ~ 16M ti00 1 200 1000 Soo p00 10A1, a00 200 2.90 0.47 0 .80 6.82 7 83,6.10 .00 73 2 3 ~ 6 0 7 8 0 10 11 12 13 14 16 16 117 Tim*. mi n Exygen Research Page 36 of 110 p . 37 Interim Report #23 - Analysis of Sediment Samples Exygen Study No. : P0000760 Figure 5 . Typical Calibration Curve for 13C PFOA in Methano l ~ 6~zeoeu a.a . aPe ..~~ r3c rro,~t u..r R~r..+on ~~ ~t .+.ianunok r~ aec x . 0.0ot0 c~ - o oom) 4.D .6 4 .M6 4205 4.0.6 9.s .a 9.005 3 .44 5 3266 . 2 2-Y.6 2A .6 2 .4a6 tl 2 .2*0 < 2,00 I .9.6 1Au6 t .M6 1 .2.6 1 .0. 6 a .0ea 0.064 4.0 4 2 .6r4 0 .0 100 200 960 400 8 66 600 Co N o.nOri s n, ay~ 700 960 000 1000 Exygen Research Page 37 of 110 p . 38 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 Figure 6. Extracted Standards af13C PFOA in Methanol, 25 ng/L and 50 ng/L, Respectively , XCN2ir6t . t3G PFi1A ~~wd~NllliW7~Oirr . +awyA 2 of Ili thm e KtNEO~w~f Area ; 1iKleqwb fRilyAh Z1'ar .W 6ps R7: 11.6alw 11 .02 1000 0 !00 40D 200 9 2D-Q .40 O 1 2 3 4 6 6 7 ~ ~ W 11 12 13 Time, wi n , Xp042000-2 -13C rFOA ( 1 tanAxd) 4 76AA70 .0 auw - "wit 3 o14E /nn D+12BOOD .wit1 Aces: 26B178 eounb Neipht 249 e+003 op AT- 11 .1 min 14 /d 16 17 11 .06 3000 n CL 16o0 1000 5000- 7.76@ .40.8 .E3 1 2 3 4 6 0 7 8 B 10 11 12 13 14 16 10 17 Time . mla Exygen Research Page 38 of 110 p . 39 Interim Report #23 - Analysis of Sediment Samples Exygcn Study No. : P0000 760 Figure 7 . 13C PFOA in Reagent Blank, 0.4 ng/mL Fortified Reagent Spk A, and 4 .0 ng/mL Fortified Reagent Spk B, Respectivel y ~ ft7oMt COAAV/ l3GPiDA (LYIIOM) IliNJ7MO11w -**No/* ~O/Kk 1I ~Q~O~OaMfI 64" AIf TOiRdJ 10 .0 CL 777 ,0.6110.Y11290.13.37 14 .OQ ~ 80 .0 .4, 7 22 w. .10a 9 . e .ea i~, a4 1a .2f 17 s OA 1 2 3 4 3 0 7 S D 10 Time. rnln 11 12 19 14 1J 10 17 , ROapOnlSpKA13CPFOACOC)416.OId70 .0am0 sample 10014Ehom0426000 .W1f Anw 272G0 oounk XofphL 2.02t+003 Opf AT : 4 1 A Me 11A1 2000 1000 1 2 3 4 6 0 7 8 D 10 11 12 TiR.e .rnts, , RupON Cpk B - 13C PFOA(Ot)416.0470 .0 imu sample 11 0146 fro0 0*4000wq Ares : 210141 oouek Height 2E20004 cps AT : 11 .1 nln 13 14 16 'tE 17 C-L 2A&4 1187 1Z*4 00 1 ! 2 3 4 6 0 7 Y 0 1O !4 f3 14 16 ib TJ TpeO. win Exygen Research Page 39 of 110 p . 40 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 Figure 8. Chromatogram Representing a Sediment Sample Analyzed for 13C PFOA (Exygen ID : C0172892, Data Set : 042806D) , COMM !JC PFQA (LMtNO~r) 4lSKJTL~ wye searple 2 1wrliTiew! W2NW.+M/f ArN: ~LAS7 eoewlr Alg~IC 29t~ .OMcy~ Rl. tY.! wrrw 2 .8 64 2 .0 64 11A7 2 .4e4 22M 2.094 1AM/ 0 1D 44 c 1 .M4 - 1 .2e 4 1 .0r4 8000 .0 OOOOA 4000A 2000 .0 0 .0 1 2 3 4 0 0 7 8 9 10 11 12 13 14 13 10 1 7 Exygen Research Page 40 of 110 p . 41 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 APPENDIX A Study Protocol P0000760 (Exygen Study No. P0000760) with Analytical Method and Protocol Amendments Exygen Research Page 41 of 110 p . 42 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 E ryge. rrotoopt rnmeber P00007 60 STUDY PROTOCOL Study Title : Analysis of Pertluorooctanoic Acid (PFOA) in Water, Soil, Sediment, F1sh, Clanss, Vegetation, Small Mammal Liver and Small Mammal Serum Using LC/MS/MS for the 3M Decatur Monitoring Progra m Exygen Protocol Number : P0000760 EprfQrmlqg Gboratorr. Exygen Reaee<ch Spoesor Rapresemative : Michael A. Santoro 3058 Research Drive Director of Regulatory Affairs State College, PA 16801 3M Building 0236-01-B-10 Phone : (814) 272-1039 St. Paul, MN 55144 Phone: (651) 733-6374 ~- . Ave I ojdS Exygen Research Page 42 of 110 p . 43 Interim Report #23 - Analysis of Sediment Samples Exrygen Study No . : P0000760 Exysex P:vtocd Number P0000760 DL4TRtBVCiON: 1) ]aid-ha Kuai, SAdy Direcror, werton Solutiow 2) jam M. P]ahety. Pr;nr i p.t ]nvatiplor. Exygm xeseach 3) Michu! A. Srntoro, Sponsor Repremtafivz6 3M Company 4) ExyEm Rarwch'Quatny wzwranoe Unit Page 7 aJ 1J Exygen Research Page 43 of 110 p . 44 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 Lxy=w homcol Nmaber: P0000760 pROTOCOL APPROVAL Stady Titk: Analysis of Perftuoroectanoic Acid (PFOA) in Water, Soil, Sediment, Fish. Clams, Vegetation, Small Me nsaaal Liven and Small Mammal Serum Using LC/MS/MS for the 3M Decatur Monitoring Program Exygat Protocol tJumbcr: P0000760 APPROVALS laisi K.esui, Study Direct, Wasson Solutions 04- pa U Wa Q_ ~ lI U O Michael A . Sa~f to, Sponsor Reprauntativc Date 3M Company M . Flaherty, Principal Investi gator Date 19 Exygen Rcsoarch ~ 7rlr,r;v~ ul -crr -zo~~ ~'+8xysen R irx. sidatt . Facility Management Dam L Sltaffer, Toc6ni Quality Assurance Unit Rceeuch f 4.1 Date Pqtr)of6J Exygen Research Page 44 of 110 p . 45 Interim Report 023 - Analysis of Sediment Samples Exygen Study No ._ P0000760 Exyten Prontol NambeT: P0000700 ... TABLE OF Cf3NTENt'6 TI71 2 PROTOCOL APPROVAL, . .. ._.__ .__. ..__ .__._ . .. ..----- .. . .._ ._--^_-..___- ._ .__. .. ..___ .. .. .. .._ ..3 TABLE OPOO[11FN19. . .. ._. ..-----~.._ . .__ . .__ . . _.. .._-. ._ ... . ... .. .. .. . .. . . .. . .. .._ ..4 @~IEODIJCIION..._.-____. . ..__. .---_-_-. . .- . .---. . ..___ - . .. .. -._ . .. .. .._. ._-. ._ ._ .. ..__ .._ .. ....__S TEST .. .._. .. ... . .._.. .. ... .__ SURROGATE FiFLD SPIKE ODlelpOl,RJD-_____..__ ._ .. ...._-_ ._...----------- . ..._..... . ... ...... .. ... S OBJECTIVE 6 TESTING _ .- ..._.. ..... .. .. . .. . .._ . .._. .. .... . ..-. . ... .. . ... .. . .. . .6 STUDYDIRBChDR. .__ .. .. -------- ------- _.. .. ._ ..._. .. 6 SPONSOR Ak?RESSF7J1'AI7VF...._----------- _ .. .._ . .. ..... ..._ ..__ .__.. ., . ._ _ .. .._ .. . .. ... .. . _. .. .. .. .. . .. . .... .. .. .. . .7 PRINCIPAL BiVBSTIOA'110R .. ...._._ .. . .____ .. ..... . . ...... .. .. . _ ..__.. . . ... ..__ .. . .. . .. . .. .. . .. .. . . . .. . ... .. . ... . .._ .. . .7 PROPOSED EXPERIMENTAL START AND TERMINATION DATES . .._. .. . .. .. .. . .. .. . .. .. .._ .. . .. .. . . .. .. .. .. .. . . 7 IDENTIFICATION AND JUSTIFICATION OF THE TEST SYSTEM . ._____ .. . .. ..__ . ... . .. . . ._ . .. .. .. . 7 9ANIPL@ PROCUREMENT, RECEIPT AND RETENTION .__ .. .. .... .... .. ... ... .... .. . .. ... .. . .. . .. .. . .. .. .. . . .. .. . .. .. .. . .8 SAMPLBIDENPIFTGTION ------ _ .. .. _ .. .._ .. .._ ... .. .. .-_._ . ... .. .. .._ ... ... .. .. .. . ._ . . .. .. .. . ._ .. .__.. .. . .. .. . ... .. . 8 ANALYTICAL PROCEDURE BlllfldARY ._ . .._ .... . . ...._ .._ .. .. ._._._... .. .. . . ..... ... . .. .. . .. ... .. . .. .. .... . . .9 VSR1PiCA7ION OF ANALYTICAL PROCBDURE_. ._ .._- .-- . .. ... . .. ... .. .. .. . .. ..... .. .. ... . . .. . .... ... .. . .. .. ..._. .. .9 MSTFIOD FOR CONTROL OF BIAS . .. .... . .. .. . .... ... .. .. .. ..__. .. .11 STATISTICAL M67HODS .__.. .. .__-___~_~. ..__. .. ._ . . ... ...__ . ..._ . . .. . .. . . ._ .- - -. . . . .. .. . . ..- ... . . .. . . _11 GLP SCATFIdFJIf . .. .. .. .. .. . . .. .. ._ .._ ... . .--- .. .. - --_ . . ... .. . .... . .. . . .. .. . .. .. .. . .. .. .. . .. .. ... .... . ._. . .... .. ..__. .... ._ . .1! REPOkT . . .. .._ . . .._ . . .. ._..._... ... .--.. ... - .. .... . . . .. .. . .. .. . I I SAFETY AND HEALTH __ . . _ ._ _ .__. ._ _._ . . .. .. ._ ... .. .._ _ .. ._ ...__ . .. .. ... .. .. . . .. .. . .. ..,, .. . . . .. .. .12 AMENDAIFI I ISTOPROTOCOL . ._- ._ .... .. . . .. . . .. _ . .. ._13 DATA RECORD ICPEPINO ._ . ..__ . ._._... . ... _._ __.__ . ... ._ ... .__ .. .. .. ..__. . ..___. ..-._ ._. . .._ . .. .. .. . .. .._ . ._ . .13 QUALITY ASSURANCE .-~ ____., _ ., .. . .. _ . .______^.____ .._. .---_ . .--- ._ .. .._ . .. .. .. ...__ . ._ . .14 RETENTION OF DATA AND AACHiVII7G 14 APYFNDDC i . ANALYTICAL L>8T/10D4 .- ._._ . .. .._ ....--_- . ..__ . .__.. . ..-_. .-_-_. . ..__ ... ... .. .._ . .._. l 5 pas* 4 of 65 Exygen Research Page 45 of 110 p . 46 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 Exypa P rotoad Number : P0000760 ^ INTRODUCTION The pwpo w of this study is to perfotm analysis for Perfluoroocunoic acid (PPOA) in wYer, toil, sediment, tleh, clams . vegetstion, mall mammal li vers and mall martunal mum using I.GMS/MS for the 3M Decatur Monitonng Progt- The tautly will be audiled for compliance with EPA TSCA Good Laborato ry Practice Standards 40 CFR 792 by the Quality Awunnce Unit of Fxygen Resoarcb. TEST MATERIAL The test material I. perfluotoocttuwic acid (PFOA) end was purchased from Sigma-Aldrich. PiOA Chemical Name : Pecrfluorooctimoic, acid Molecular Weiori: 424 Lot Number: 23116HB Purity : 97.64/. Trmuitiona Monitored : 413 -+ 369 (for quantification) and 413 --).219 (for oonfamation) Structure: jj P F ~ F F OH F F F F F F SURROGATE FiELD SPW COMPOUND The surrogate fidd spiking compour,d is ' 3 C labeled per fl uorooetenoic acid (13C PFOA) and was purchased by 3M from Peridn- Elmer We and Analytical Scienax. ^ ' 1C PPOA Chemical Name : 1,2-13C perfluorooctenoic acid Molecular WeigM: 41 6 Lot Number. 3507-195 Ptvily: 97y. Transition Monitaod : 415 - 370 Pn9. s of 6 l Exygen Research Page 46 of 110 p . 47 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 Exysrn Prow" NwrAcr P0000760 .~-- OBJECTIVE The puepoee of this awdy is lo perform analymis for perfluoroociamic acid (PFOA) in watet, ooil, sedimeat, fish, cMa, vepmiom, mall mammal livers arid sateU ma~ tetumt for the 3M Decatur Mooitoria8 Program using the cwrent vpoow of the followirq; HzySea welytial method: V0001780: "Method of Aualy:ii for The Detamafuion of Pstfluorooclanaic Acid (PPQA) in Water by LCWWS " V0001781 : "Meliod of Analysis far the Determination of Paftuotooctamic Acid (PFOA) in Soil by LGMSlMS" V0001782 : 'Method of Analysis for tbe Deoermiaalioa of Petfliwrooctanoic Acid (PPOA) in Sodiuxot by LCJMSIMSV0001783: "Mstlwd of Aeatyo& for the Detarminpion of Perlluorooctanoic Acid (PFOA) in Fish sod Clam by LCJMNS' V0001784: "Metbod of Analysis for tlSe Delamimrtiou of Pafluotooctanoic Acid (PFOA) in Vegetation by LCIMSIMS* V0001783 : "Metlod of Analysis for the lhtamioetian of Porfluorooctanoic Acid (PPOA) in Small Mammsl liver by LC/MS/MS- V0001736 ; "MstLod of Analysis for tbe Determination of Pcrfluorooatazwi c Acid (YPOA) in Smell Mammal Scum by LC/MS/MS- TESTING FACILITY Exygea Reseercn 3458 Ram=4 Drive State Collage, PA 16801 Phoaa (814) 272-1039 STUDY DIRECTOR l43iaoba ICeafti P .E., D8E Winton Soltttiom brc. 1400 Weston Way Wed Cbvdw, PA 19380 pitoee: (610) 701-3761 Fax : (61D)701-7401 j kesvi~watooeolutiotu .tw~ Pop 6 c163 Exygen Research Page 47 of 110 p . 48 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 ftypn rruexa NmLer : Poom760 v SPONSOR REPRESENTATIVE Michael A. Sentore 3M Cmipany Director of Reptatoty Affairs 3M 6talding 0236-01-5-10 St. Paul, MN $5144 Phone- (651)733-6374 PRINCIPAL IlVVESL'IGATOR John M . FWwM Exy m Raarch 3058 Reseatch Drive State Coliegq PA 16801 Phone: (814)272-1Q39 jolut.flahertyexygem.com PROPOSED EXPERD&ET1TAi. START AND TZRAMATION ,.. DATES Is is proposed that the analytical portion of this atudy be conducted from October 01, 2004 to December 31, 2005 . The actual experimental rtut and termination dates win be included in the fma1 report. IDENTIItICA71ON AND JUSTIFICATION OF'f'HLTEST SYSTEM The following we the teat system for this study: Wata (groundwater and surface water) Soil Sediment . Fish . Owns vegetatiott Small Mammal Liver Small Mammal Serum The samples will be collected by Weston Solutione. The control samples will be purchased and papered by the testing fiei6ty. Purchase and processiN Pao 7 q143 Exygen Research Page 48 of 110 p . 49 interim Report #23 - Analysis of Sediment Samples Exygen Study No. : P0000760 Exygen Protocol Number. P0000760 0 ,1 dotai4 &x the control samples will In included in the final rVort associated with this study . The tat yens we chosen to access the environmental impact of PFOA in the Lkeattu. Alabama area . SAwLH PROC[3PARdENl', R9CMT AND RETENTION Water, aosl, sedimmb M , clam, vqdatiam, small mammal Eva and small manmul aatmn tampla will be received at Sxy`oo directly from Weston Solnboos. The detalla of Sam* Procurement for this study W* oudined in UK 3M wodc plan entitled -Mew 2 WorY Plan for StLropliaQ Environmental MeOia." The number and typea of samples collected will vary depending availability in the field. The total twntbei of samples received and analyzed ft each matrix will be docunen0ed in the final report associated with this study . Wata4 aoil, and sediment samples will be used as received without further processing at Exygm These aamplts will be stored refrigerated at 2C-8"C . Fish, clam, vegetation and small onunntal lira samples will be processed accad'cfs to the apptopriate analytical method pee Appendix i) . These 0.- samp;le will be stwod frozen at 5-10'C. Small mammal whole bbod samples will be centrifuged in the field at the time of collection and t he serum fraction will be used for to study . Small a>aataoal set= will be stored frozen at s -t0'C. The receipt and procrasioY of the samples will be documented in the final report and raw data associated with the study, SAMPLE IDENTIFICATIO N Prior to aaalyw, each sample will be assigned a laboratory sample reference nrmbec. The reference number will be mtiqoe and will distinguish each Iabontory aanpio do is pmaesred tb[oughout the analytical procedure. Chtomawgraphic data will be identified by the laboratory samplo roferenco tu ubac. Sample storage conditions and locations will be documented througlicut the Study . Page a of 63 Exygen Research Page 49 of 110 p . 50 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P000076 0 Eaytn An~oeol Nw~er. P00007E0 ANALYTICAL PROCEDURE SUMMARY Referener,s: V0001760: "Method of Analysis for the Determination of Perfluorooctanoic Acid (PPOA) in Water by WNISUS" V0001781 : "Method of Analysis for the Deleaeioation of Perfluorooctanoic Acid (PFOA) in Soil by LCIMS/MS " V0001782 ; "Method of Analysis for the Detcrmarrauon of Perfluonooctanoic Acid (PFOA) in SetB.r.ent by LC/MSJMS" V0001783: "Method of Analysis for the Determination of Perfluorooaanoic Acid (PPOA) in Irish tcd Clams yy I .C/MSlMS" V0001784: "Mtt3od of Analysis for the Determination of Per(luorooctanoic Acid (PPOA) in Vegetation by LC/MS/MS " V0001785: "Method of Analysis for the Determination of Pertluorooctaooic Acid (PFOA) in Small Mammal liver by LGMSttM S " V0001786: "Met6od of Analysis for the Dotarminetiqt of Pcrfiuorooctanoic Acid (PFOA) in Small Mammal Scrum by LUM&WIS " The above methods use analytical conditioe : capable of separating the isomers of PFOA. The final report will include the isomers summed into total PFOA found. VERMCATION OF ANALYTICAL PROCEDURE A laboratory control sample Will be used for the preparation of fortified oontroi aamplet The test substance will be made into solutions as per the melhod, and added to the matrices via a mieropipene . For water tanpliag, Exygeq will supply one bottle per sample collooted . The bottles will be 500 mL precleatxd ScilSPec Premier wide mouth HDPE bo ttla. These bottles have been routinely wad for PFOA ample colla tion at the testing facility srd have been dawn to be free of PFOA. All oontainets wed for water simple collection will be shipped to the sample location corpaiain; 100 1118 of 13C PFOA (oqtrivalent to 5 00 oyL in the final sample) . Saioplw w ill be added to adt roatwnar to s vol=110tric fi ll linm at 20 0 mL A field duplicsoe, a low field spike w d a high Eeld spike of each srrqyle will be collected. The low and high Sekl spikes will contain PFOA as well as PerRuorob~ls>eailtonate (PFBS). te (PPHS), and Pertluorooctanesulfrtaatc (PF06). These compounds we included in the solutions used to spike the samples . The results for PFBS, PFIiS and PFOS /" will not be reported in this etady. Exyi= will supply one field blank (Control water) and two field blank spikes (cocnrot water forti fi ed with PFOA at a low Pays 9oJ6S Exygen Research Pagc 50 of 110 p . 51 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 Exypm Proweol Muaibn : POOn0760 and high level) for every twwty samples oolfected . At the testing facility, each water sample (eaeehidina fold duplicates and field sp+lces) will he extracted m duplicate and will also be fortified at a low and high concentration with PPOA and prooeswd due"& the described procedure to dlateimate taatbod accuracy and to chock for bim . For soil, aodimmt, eiatm, sad voge.tttion, Ezygeo will supply one 300 mL precianed SeilSpee Premier wide mouth HDPE bottle per stunlite collected or a zip=al bag All coNainanybogs used for sample collection will be shipped to the simple locattioo. StmpEet+ will be added to each container or bag in the Geld.' At the testing fidTity. each sample will be cKbWW in duplicate, and will also be fortified at a)mown ooneentalim with PFOA at both a low and Wait level and processed Ihewp(t die daetibed procedure to determine method accuracy and t o check for bdur. UGPFOA will also be added to each sample in the laboratory prior to extraction at the level specified below . For ,mtall ammml liver, Hxygen %,ill sapply a 30 n2L polypropylene centziflrgn tube. For small mammal aauut, Exygoa will supply a collection kit for each sample cdanioy mine separator mbee (red top), vacutainem needle holders aed ueedkt, traoafer pipettat, and polypropylene tubes. At the testing Gtility, each Mm and mm sample will be extracted in duplicate and will also be fortified as a kown concentration with PFOA at both a low an d ~,. high level and processed through the described procedure to determine method accuracy and to dwelt for Was . 13GPF0A will also be added to each sample in the laboratory prior to extraction at the level specified below . Low and high levels for ea ch matrix ars defineJ bslow : Matrix Lvv PFOA High PFOA CPFOA YVater SPIMM Level SW U SoMm Level Spiking Level 3000 n 500 n L Soa 4nW& 40 aWlt 40 ngig Sediment 4 40 E&g 40 njr/ g Fish lonwg 100 n loon clan 10 100 n 100 n yeefttion 10 )00 100 n Small Mammal Liver 10 IOOZWK 100 n Small Mornmg. Sam 10 RmovaiM we anticipetd to be betvena 70% and 130% of ihe foniSed leveis; )rowaver, At exact preqtioa sod accuracy will be determiood by the analysis of the quafity control aanapla described above . A statement of accuracy will be included in be IIml rapom Prior to sample analysis, a labOrMory control apilca study will be oonduaod in ~~. water to justify IM we of 1rC PPOA results to eatabliah precision and accuracy of PFOA samples. The following samples arc to be prepusd : Paz, /0 of 61 Exygen Research Page 51 of 110 p . 52 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P000076 0 6xy<ea Prorocol Number PODW760 TWO control W*W blanks TWO cosiIIVl walar samples fbtYifietl ac 250 npJL. with IrC PFOA Two control water samples fortified at 250 ng/L with73C PFOA and at 250 ng/L with "OA. Two control water samples fortifud at 5000 a8/i, with "C PFOA and at 500p ng/L with PFOA . The above unpin are to be extracted and analyzed according to method v0001780 entitled "Method of Analysis for the Determirmtion of Pe:fltwrooctaawie Acid (MA) in Water by LCJMS/MS . METHOD FOR CONTROL OP WAS Control of bias will be eddreaaed by liking represeoueive sub-samples from a homogeneous miuwe of each ma trix from untreated Control sampks. and by analyzing at least two levels of fortif.catians. STATISTICAL METHODS Statistics will be limited to those specified in the subject methods and to the ealculation of average rocoveries, as applicable. GLP STATEMEN T AU aspects of this study shall be performod and reported in compliance with EPA TSCA Good Laboratory Practice SUridatds 40 CFR 792. The final report or data package (sapplied to the SpoQsor) sball contain a statement that the study was conducted in wmplianee with current and applicable GLP stmtd uds and will outline any deviations in the study from those standards . This slatamoR will be signed by the Study Disector and Sponsor Reptesentativa REPORT A final report will be pnepand by the Principal investigator or their designee at the conclusion of the study. The report will inclnde, but will not be limited to, the following lo~ page ft of 61 Exygen Research Page 52 of 110 p . 53 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 Exnft Protocol Nuniber. roooo760 ~. . . The name and addtrsa of the Study Director, Sponsor Rcp ssentstire, and Of d e testing facility. A qstaneat of d1..P complia= ( any miallod such as chain-ofeuotody tocotda, man be in the study records) . . The signed and dated atatameat by the Aatygea Research Quality Atsarame Unit reprding dates of study inspections and dates 5ndings wese repeated to the Study Director and MumBecient A docaiptian of to act analytical conditions =Vgoyod in the study . If to subject method iraE ta0aw ed ncaetly. it is ueemsary to include only a copy of the analytical ansmod. Any taod+5casiotq to this rualbod will be incorporated into the oapoet . IS the method it photo-red.ced, the project number and pap samba must be included on each page. Description of the ins>mnnntation used and operating conditions. AD results from all sets analyzed. Control and fartified samples will be identified and the data table will inch* sample number and fortification level . Representative eluomamgr>tina for each analyse in each tnatrix, including chromatognrna of a atandad and s cooao ll sasiV ic, and a chromatogram at a fort3fieatioo level. The location of the analyse peaks will be clearly identified in all ebroaaWgrania. All circumstances that may have affected the quality or integrity of the data wil l be documented in the report. . Lacations where raw data and the 6nal report are to be rckrivod , Additi ow a corrections to ft final report shall be in the form of an aaamdmari signed by the Study Direator. The amendment ahaIl clearly identify that part of the report that is being altered acd the reasons for the altptationL The amauiment wiU be si gned and dated by the Study Director and the Sponsor Aeqmsattative. SAFLIY AND HEALTH laboratory personnel wilt practice good sanitation and health habits. Every retmotrble ptecuttioe shall be ukast to prevent inadvertent exposure of paaoiael and the environneet to the test or reference Cu-. Page J1 of 63 Exygen Research Page 53 of 110 p . 54 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : POQ04760 Exna, ProWr.ot MUO*er: Poooo,bo r~ AMENDMENTS TO F'ROPOC4L All aigoificaat chumps to The analytical prmtoool outlined hem will be expressed in wtiting, aigoed and dated by the Study Director and Sponsor ReptppAativo. Anxndtneiw usually vnU be issued prior to initiation of study plan change . However, wlteu a chap it required without wlLcient time for the leans of a wtium amendment that chmgo may be effected verbally with supporting documentation aped and dated by the Study Director and followed with a wetfett tmfendtnpn aa won an possible. In this caea, the effective due of the written aaeodtneot will be the date of the ducumented change . Copies of the, signed arsandmano will he appended to all dietrtDuted study PING copiea. The original ataendtuatt will be maintained with the oriptnal study plot. Any deviations from the study plan or from the analytical method as provided will be documented and reported p-tpuy'A the Sponsor Representative. DATA RECORD ICKVING Records to be maintained include the following (aa approoriatc) : Sampie ttackiny sheet(e) $ample receipt records, stora ge history, and chains of emstody Hietoy and preparation ofetanderds (stock, fortification, calibration) Description of any modificaunns to the method buahutr e nt run sheets, bench-ebeets or lop Analytical data t ablea All clmoouqopapAie and intnumettad caitlitions Simple extraction and analysis dates A coatptete tieAng of study personnel, signatures and initie3a Chronological posents6ort of all study correspondenc e Any other doourna tMation aecex+ay far the reconstruction of thc study Chromatopramt- Al chromatograms will coetain the following: . Simple identification, injection date, arrow or other indication of the area of inirseat, said injaaia number oorreapoadmg to the run. . Additionally. fortifications will include the amount of analyte added and the sample number of the simple that was fortified . Analytical standard daroanatogranu will *dditignetly include, the coneentrstioa (e.g ., gltrL) P a s s I i cl6s Exygen Research Page 54 of 110 p . 55 Interim Report #23 - Analysis of Sediment Samples Exygen Study No. : P0000760 Fsy;ea rrancal Number. POOOO?eo ~ ., . As part of the docommtaloon the following Sheets will be included in each nialytical sa: s run sheet Win the mmples to be an in the t+at, sad an i nstrurnwN tooditiau sheet dewribins the instrument type and operating couditiont. All applicable raqunanent+ for reporting of study results as per 40 CFR 792.185. QUALITY ASSURANCE The QA Unit of Bxygm Research will inspect the study at inwvws adequate to aaao+e compliaacro with GU's, ad will repeat the if u iaps of audits to the Study Director. Paryra Mioagea+a k and the Sponsor Repmentatim RETENTION OF DATA AND ARCHIVING All had copy aw data, incltAnQ, but not limited to, the original ebtomttogr-ua, warlnheeb, oorzapoodmce, and results sha ll be included with the data package nbtmitted to the Study Direelor. now will be archived .~' with the original study pltn,, aIIteodments, fiael mport, and all pertinorx informalim Rom IM sponsor. The testing facility shall keep all elec7rotsic raw data and any instrument, equiptueat. and ttasge bP for the Period of time specified in 40 CFR 792.195. An wet copy of the materials submitted to the study director will also be kept et Bxygen Reeeach F.xyy will obtaia penniecion from the study director before disc ardimg or returning samples.. Pop* )I of 63 Exygen Research Page 55 of 1 10 p . 56 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 6xyjeo Proioee( WumDer. P0QW760 APPENDIX I ANALYTICAC. METHODS V0001780 : "Method of Analysis for the Ae emarinetian of Pertlwroocwroic Acid (PFOA) in Water by u.Us&s- V0001781 : "Method of Analysis for the Determination of Fe rtluonooetuwic Acid (PFOA) in Soil by LC/MS/MS" V0001782: "MctLod of Analysis hr the ,7damtination of Perfluorooctaooie Acid (PFOA) in Sediment by LCJMS/MS" V0001783 : "Method of Analysis for the Detemninetioa of Perfluorooetanoic Acid (PPOA) in Fish and Cl ams by Ifi/MSlMS" V0001784 : "1Hethod of Analysis for the Detannination of Perfluorooctanoic Acid (PPOA) in Vegetation by LGMS/MS" V0001783 : "Method of Analysis for the Detamination of Pertluorooctanoic Acid (PFOA) in Small M==W Liver by LCft&.%/MS" V0001786 : "Metbod of Analysis for the Determination of Pertluoroochnoie Acid (PFOA) in Small Mammal Serum by LC/MS/MS " Pnpe 13 of63 Exygen Research Page 56 of 110 p . 57 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P000076 0 F xryBea ProlOOO( P1uruba: P0000760 ANALYTICAL METHO D 1i16 IKeYw : Vo00t710 U064stM OP1 4IM nwrAl.wr. d?a'f VwMeswl . Adl (!7'OAy 1s wn.r by L~'J~e W Aa 4ft a1TwbAI lriLq: hl'/a >ArrrJ Su6i Prewsb Drirs SuY QlL/s, PA 1610I ` ~u C.__11 4 1r..1rC:.a. c..wo .. w+is.l my"t a O.r .R ~~~~- V~ r,. WN ovWM .6 m~,M. eMce Ak~r~~l w. Told hwr: 7 for !Q aj6S Exygen Research Page 57 of 110 p . 58 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P000076 0 ~ Ex "M Proatd Number. FOppp760 N'~~b bYWM.Wrvelei7b A.YALYYICwl MITR00 1(e~oN dAaJlv>Jt me IfAe~NropvyNek Atl0 (rFDA) i. M Wr by L4L416 1 .0 sow Aw RAW is Y N 11o wt 4r so wlEtiw ~d N MdjOM ot ydk~sworos ul! by MO HrYWwrrr LW" CbsqwtlNi W NN7Md is i ondwN ?la.. A~*~r D~Aor (LCAe+ti~ n .sr. 2.e 111" LI A1..2. ob~N 0-6- on~Ney}nedea 23 GrNk6N~p~qti~leMlDlONlhuMupie6ArydaE~t6rpapv~{uy ~er0o~~ 3.0 f^bqqrivR= t 1.1 Al Yr N sL Ntyw Sol* hr a 7.2 !b qbNts.-imO Y rdN Iw ww .,IM a.NA. Mow6 ne+sww r .d0 M w...6 10 .puwwe oe pon "mv.u.+. 3.4 All =*= aAd be Maryty a4M6 MEw b -W arqld fer aw~crion 7 .7 Any 1Nqls aaWm{ 1 " dN dpil6 bs arfAF6 N[ -3000 ipiu M-S ~>r -1 tl. . Mmwrr MW tw on .M3 .4 Sank miNeaM r oertis Will be 4K09 6 in as SU1p1u4 yLn Wt., P-q- 40 l " wY ad M-1~ ll WNINr-IRLCIW 4.2 LLdAd-IOLCNr d. 43 A~ Amt ft -ACS.1apmICn6o 44 Msmoctooic Arid- > P r4 1* leA 10 Lmonl wd 'I pp.ot 5.1 7-2 5 .3 5.4 !.S A 6i* 1M 61 M dr MwtMpa tNrb4 of pre~ ~y is 7 MMU SOW" so r wi I li web = b*PN r eytlN of itqayU 5200 Lmr -Md IM 4 h wdm Nw 1tNNMrMw .CALLbt11 A6mabdslao .rYleprkiY~.oosN.6~ppov~ AdliwlLloe~rW~[mAq~~o0.00101 {, SO ULY~p~WNN31 orylMaMffyewWa /f -1. AyM- r Pd1FNIflr OriYP Ob. u ~9~4 s~(M 100a1 . 106Q0Da14 11 127-=1. L1YII aeor .se ah lodr Si 2 n1.dsiiP7C~idHt. 5.1 DUP." pprya, 5.10 Mrp}rN n IN0U00PLr IP100tL), .ild~~byti0a, ill WOM ]'Itit We 6ae 0 8) CINtP6croi6pp. y1vl ' Pagr 17 qf 63 Exygen Research Page 58 of 110 p . 59 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 r.zyIn PAn,ocol Nuaber: p0000760 T,n. .~--+ r....>a.~ .. wnAo AhALvncu.,srao. StAu"M metrDwrmlerfo .UMlrwomrN.AeNCroN .Wrrey 112 9s ..e.r .dw. s.u Q~iMOpubw a[yiMing 30 aL7olypropyirs mbr a MO q.. s.o a.a ..r vIPrl.sy.., f.l Antylier C1it>Iw lkes6w 1<? PG)wao Xtirrde6 t10 !0 ww. sy (ar:82505-msu m ai tMrM arc 63 WAIOrMwNl : 2 nNAssoACewia W4ftr c.a wbirtrM) : 760..t 6.s dr' .o l1er Flo* PA98 1foalniU !LA XH fmLaffisl OD 65 35 aI 14 is is 0.3 eo a 7s 6.) ]0.0 ts 1S ~.) 225 63 33 0. 1 to kjOtdpoValnoc ISrI.kw boinaNbrnalrSDyL). 6.7 Q uEN 1 6o; Mt/wo-a~1~WiLnYmevne N Rs7i w -77rrwa ~ ~ An u6 pd4 rdmryMshayeduoNa a 7.0 WYI{i 33atf 7.1 ilcic 41q.~wf N.~n 1RN ~odowadriY s IS -. 761 ndi. The row OIdYeY w ismdd r~ yade rd Op11G M BiD vq/ a a n.rr; .rw. ..~ u w7. K., . Ay E. d_pd r adv p i1 .1 t al[ w, prio oW i wrr u preprod by W iio6 Q I54 r of rosb b 7000 wL W vrw. Aue~w wll Wra ey be poorei nr~ I .r= P~~ /d Q/'63 Exygen Research Page 59 of 110 p . 60 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P000076() llsypn Praxd Numb.r. YOOOp760 00. .. w+wwr .veo.nw A[bWY~1CAL IR7IIOD . Micd .[A .irw irlM DM .wiipiaq ~ AM "OA) in Waw by ll'J36AIS to !111M vlY,rirl.a 9.1 !In/ .dA.$7~rWe~tiaye~i~ 9.1 .1 h~.. . .rlwalva-lawYar.an~oAy ..;~1o,.Y ~~~~b+ cwMtw ta~ Y.+r) d 67.! r loo aL wMn mob" r . U5-at L.6 brb. 9.1 .2 AIO "Ad.YMpdq .pinlYAe(pNAYpqir9Y0yprMpylu s1. ot IM 100 POi.L bMYlaa b . Orl ral .e. ot 10D wuh w<erd in .llf bi .lDN MYM, A1A WMLLn Ow.laswlwaad rOAitpaa yerfnq .1 n, +idM 101y~nL w1 .6e . b .8.d .~Ier d l00 ~nu ,u, .,.o~ ~o 1127 si. GOrE bOM 9.1.~ A 0.1 YriL rd 6..dw ei .i.. .f 1PlQA is prRr~d by 6ri.yy i n a[.4f6 . 1-0 MdsL . 101im b.le.l yduAy of I OD rilY weYrd in .1f! =1. fLllYe. 4 9.1.1 A A01 POOL h"wtiw bl .iq Ol?/OA is pqn.Y ~y b~i1Y I$ d. of Yx 0 .7 rwL I . 10 a 0o.1 WON" of 1 0o w. WOOL .rYlaSnLDB 9.1 .a lL10 k m d 666.+.. el0i.b a o to be IbwO in it r.6ip.4r it bpmdbMi) f'C . .0 M wbN IN s . P iW ot! nwuna i.w d .2W Mrqrnk~ 9 93 &a.rrd QL1M.n MIppp.q .21 LOMfIAY o4t11141s ~..dWt an pb.r a NPIt' ~u Th. "aw"O" M ~rbd ~wyi b. nb,ctiw P ocduc. iY 'ml b ~ 9u r boomb* .7M41 a~ .W.c .Aalf...l w~mmtlon ANY D . w . Fh Oaews hillrm - V.L. .f G ..wwla at am. o~laYhYb Vul1 M lw llld6Y.1 4YL.ti.1 Swodrd ID ~0 9 10 1M 40 7! ][C1.~dpf,1 t0 7N 40 H 1. 4IY Y ISO x~J 100 3" Y no Xp-ftWn, I00 70Y 40 740 ZmW1yJ _IYG 400 M to" 1[p .00w; ' T!. Qrra ea .smdea KO. e.W.Ya~ql.r. b .MM 1. Y. in irriid --ow"IJ016 - . s.vctlw (SrE). XC ~wlLirra~iai. ~~~Or0 Ariy Pw 7DaJ6S Exygen Research Page 50 of 110 p . 61 Interim Report #t23 - Analysis of Sediment Samples Exygeu Study No. : P(}000760 80'tro PNI" Numk, : Po00m6o ~. ~ji6i"~ r..d rr..ewi~w .IYALY7JG,., V4YDD 1Mb& ITANUpw biM DwrrYW~ 6CJYylt br ft~ A a~ Mdrt wtr6a G~~r 5fsq r~ILL~qr~d w th wU rt draYi wanr.i. 9S4 wow ~l at~aMd talLWea rndrb ia 13aL Syy~ap~ ta0a r]'Cri'C,yy~wMp, f27 A1Wru xMen r~ owea~eYYY ef Wri aqr 6t ppral u r~dd laa e.lebsrt7~ RIM 3d MIA .C + Mlr . ~eaw/ p P Yy 20 Of law) MR ioclW. r 1a. tr "No eaaYUl 6rwbd tiLL -no l9Lt w.rrl M 6 me rhwpra r 01 0L 60 W/ as Epa rarCaurr (bb wMCI pltq n vpi wedw+vYlr0ralaa pir 163 Rvyi u rlY ir MM MA Wtlsy *49eMr W Milw VAN Ie qaeiiod ib 9diy rwrw 31r Lr Or. Pqj.a 11-0 88116 P~rea 11 .1 YWA a 4 OrLKfmpUata psasd s"YSlYa04 W aii .wA wwr ~~/a0l~a171M -*p (!M!y Y OMJr~ -pi. iftl &A ] l .i ONO- i Gw S!! ptollra (1 L 0 14 by Mft 10 ML rr*MW W)w .d * f =LdlalCwprhidycl DoaMMaYm M dry 11.7 LaMrrprataaiiwdcr,lrIIaa WO Diquddpb. 11.4 Rrr with a ML U0R r913rW. Who s rL or dab i.r Ordrwd 14f A WW". .) -sd w a~tf 111 DOW ia rwa arunl dal nkwA,d. rr'M ad btle .rqM wm Me WNW" CAM A =11=W rnrrf sr pr.a~s rd Mlw. rl MINNOW r ns la 13.3 ierii~ id` A a~ r M Lrt a" or rw~ eeaaMosoar Mwb IZ3 A. r6s ar a! rbrW ="m MA6.0 .0 b. j.~ r ~ MjriO ud r ra ed of a men* t aataaad rrb * arr I. YWWrw 164wN ~Y 5- 10 Mrplr Al r ahsrwk ft rur. - or - b~~ o! a ~r leHowM )rl ~wM oYMtMa ~i adwrprr n~d r,nq' 11 D Maqtw ('a a a ar 6 a Mead a1d -La+rrf WeWb ft -M- qr. rm WN! w1irM rrr+aat M LW Am ad 1r[ iwJr,tiea in a wwyM rp. 114 WO liw w.A.a 4m he w:+ .L L. . .wr w.a .s Y-nd b ia -al)u by War iy "ioa yiK lh w i~ d ,.k y.a ww sd , Pq010of 6J Exygen Research Page 61 of 110 p . 62 Interim Report #23 - Analysis of Scdiment Samples Exygcn Study No . : P000076 0 HxYem Ptotaeol Number. P0000760 s,r. w~a M$+W*A* . Voai 7w ANM .1f17CAL FRIIWC N66o6 a(Anlp4 Jz tV Dp~Yrdoa JT A . A Aeid (MA) in WSWO), 1 .d1iW11! wM4 OW1qWw aIdW - Wft 514eY.yu 9 331 w r4 wska) a &WOw I 12! 6sp4 "*DOW rYwid aa "MM AMd-d -W-M . A., _ -WW lb. ata0 -nd wd aymwa MN1dM McaMW wd dpN. /~ ua 0.0 MeMwOAr~ 13.1 (Sw~dk f4w ~rt ~ a~Mk ata daz~M4r iw a 3Y ars 6~an a paax aL4L1 a Tie 413 rr'rut eawap W Is llr Pr'OA anwft wbk Ae M~yYwiw OA .~) Aw-wk tp . b. .r .bboi d.. 117 1M4od bIWu ONO wt mi in 1FOA it b 0 rrr tM &*LOQ. Jr . limb ae M kW i10A It kWYW /a7" 1W 1W SO yM1 , do a MW b" me** awb er`m a ad iw riw ay r b W atMa.d 13.3 {4wwfat afwal Wl;m a/ arkiet "am r 1s IM~rw TtUOfL or st .h '.. N . 00".+ Wa. ek woa VW +arr1 . rwr, e 9 +n A Of ar Plat iwld M mitt Mry .W. V4. owwM 7.0 luo% rodl is woad by rr auyt k w- i ir .asr.aan n r.mMd. 13 .4 AmW Wa Okaid 646 M M a dk54pa1 opykr by a" *. lly Ow TEL r4 M swMM6 Dw d eYcritls of an eYitraaa cw, IiwiwR M M{ -OM of afeokd adiatia wrdri trt owdd hs am*" WM Ml atird W% of am "W womb. of Wd.,6 Iqikd 71. ..wrr ..~wr (A1 f r =&"w mw O o.ws" Ow b. am m me* A. - al' aaftf~ 1t WIirY au oitia. s.e,a o " MM is low MU qppiw w rr Is iaa rt pnfo ., r tlrc Mdrd~a d wk~t d of+oPl~ ~Y.nY /e ratu0aad. 17s reries - b- -id w4 rd reeON nnr .a driA . Na. 44 %filwl a -b dtr ML 1(e ~ tI w Ylt afq00t Ilu IiwM .0&M 4* wtyucd ro daa iM w not be rwnlyNd. 14.0 G1wWM 14 .1 {IM IN AOCrft Nrda tl uk7ip- Ib rMrM O(}ypA rfted i'+rY/L. krM af prlc aw) uo" so M wdwd erw ( i+w rarrrou vr .meKn, pr~l~dtir tL Itrm t.yiu &~nc }io0~ "OA 8ed Myl.) - 2aic .r . ~n~so.en a pp AM Bf - L1RW y MLY 60 id *dw. . w dOiaW . Ir mo.muy . rue4Wl Per 11 of 6 J Exygen Rescarch Page 62 of 110 p . 63 interim Report #23 - Analysis of Sediment Samples Exygen Study No. : P0000760 Eayre Protood Nwvber P0000'J60 ~owe~ r.~r -b. varim aIYM.YHCAI. MZTDOY ~~ hr 20 Dw~r.a I .O4aM3 .wU (lTDN i. Wow r MI Iv a mVir ft"" +di lowM ee08 of 7RA f~ 0 aawmen. u r ~ri N~m ridolw ~r ~wost n~or~y. rdd]r &rd(ah.l wbw buducardOSL)l 100 rl~dhi(~] hp M 'r~ Page JJ vf 6S Exygen Research Page 63 of 110 p . 64 interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 &ry{eo Protowl Numb w. P0000760 /"' ANAI.YSiCAt. AZCHOD YqladNrW V0007711 JIW40 ~lAr~b /~ fM D~aeobrN~ dtii0.wwesrMe Asa (rFOM u aw ~7 LCMNti Asb 6lT.e:k5 *,dy ft"..a ..Rs 703t lun.tal Afw A~ G~ PA t6101 ImOAwO 8y ~i.-.A Pml C rsiy Tog*" Lw., calu, MtMw Rama lo k4104 DM* Pw.a ~ ToutP.rc 7 100- Yato l3of63 Exygen Research Page 64 of 110 p . 65 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 &ryM Pralocd Nirobw P0000760 ~M~+ iwrarrsvowt~t ANALYTICAL 66TYpD WMI ofArly~Y wrDr~arrq~fhdl~uoscrwk Mid(MUA ) h 969 by L('MY B 1 .6 so " lfi Mm"d V U M 41spd 6 tV irYfa W~1iYri~n of pwlLwtooewoic d by AiM Me - Li "d pAmro pvhY w .pyd in r, ta~Mrro Muc 9~aa~tr's DWelar CJIOI1fS) a ril 20 sea " 2 1 Ah dr olrewrh yareryNea4a S3 C1 MdlArrarywrWsl a- bfp- Armks +ry A- isdfw^opvsiey 1- 1a f~4 ~ ).1 A8 lwlfA 9ftiarnpY tz ~iaOm 3.2 1b -M bASe-i" i w ddlr~wl PIw. 7J W. OIaM r~twi rM6 be Yb~nO to fpwiNms n cwm WMVftdwL 7.s Alm0r~MMaorg1y drd 1 ~fa~MiK unpW finear.cra.. 7.S 50 p 6 abpw ~ir +fi l~ gwW m i~ aePliy '4n Ar Or . /N K t0 talp Y a i 41 WOW -IQ'6Ctai 4.2 1hOd- HP{GSrtN Iu AMMerrAr Aorr-A.C.i . 1nPM QM 4.4 Tw6nw*y=@ 1 Ad - SirrAl6ieL s.o r. ...M aB,0.r it A o pYrr~ 11 ri/ ~nYSVpp ~Y~ of D~W~i nh li ~~l Mr i wd,W oet+o i4s+or a" ot ;qsiq ML m~er~d ws rMr!4w 3~sewu ILCJKSMSl S.2 A4Mr o wdm iwrlyd4 prtk~ m9uryruan f .] A-yed Eolro. e1plbh a(.64 b .00DDOl g 5. 1 30 -L i09=bb polWoplr aWifu, V "b. Ss !s r[ . A 1 p1wiM P1)PM7 Np ivba s s D'r4owsw"e. (m 1 oo.1, soa20o. ,.3 . s7 175..L Lon ewie.+onkb" 18 2sLdwMlLC .iMIa. s.s arp.rw'ip M. SAD AuuDiprlrpDD.tDDOI1. od1D.tODyC),wimArrporDlL 5. 1 7 rrw 3yh9vr6a(1 1) .CIa6r8c.t<idatf sa .. ~ rr,Irla 1s1,2 Munk bMIL 7 to z s-]DO w : .rt Post 24 of di Exygen Research Page 65 of 110 p . 66 Interim Report #23 - Analysis of Sediment Samples Exygen Study No .: P0000760 /- Exy=ea Promcol NUmbcr. Y0000760 6wwrwa wr.+n.r . wol n l ANALYUCAL AlN lilos A) 4a so,t 6r W~ 9.1 4 +M916400a Z. l.1S CrtiMV aMbMo{ opimiryf0d,pNwW7la abase S000 rpm LO f3lmw-Owtleyv- 6 .1 Arl~ Ctl m TdeoYr AP as RA! 11Im4 621pJ 'lfOPMOrr WIC 63 1MbiblYwr (A) : 2 wM AeAeft we AoAsr is Warr {. MAIN ,1I.m ! MMOW ss cltaamch ., .` a So owes. 5j, ~ SA ) i6 63 6p ?3 lao 25 as 6s M MAP flowSK)IM 3s 6.3 75 6 .) n e.3 u oa 6.6 i 016" Ve110! 1l,1 .(erNYi01M6brtme M70PL}. 6.7 QuaIIdM hIcMM-~tOw~1~Y~Gs~wh'Mriaaca .. 6.t IOrTLc - 23dsor . 7L 4 lwM Mi161rw btmd me PAD d soy b du kpd in adp to 0011tal do fine 0110111 . 7.0 WAS aymesse, 1.1 Mols ENmsp~sy N~puw 1~>t wNc, ronit .oH I I3 - . 369 4h fw 1'FOit AM *m anliuor v s UIVW r a pi4 aid may be GLmpd io "to to ~ M HSw syA s. IIA twprww KS0Yiiw e 6.1 I/s1Y67Lr L11 2 d( wnwdr saob 1a wow b ppro1 S7 de4af 0 ISa S of wwws wIM oP IDOP oL ol rra. Ahww xMO~b vi' De Ripas C. Pa;e 2J 4( 65 Exygen Research Page 66 of l 10 p . 67 Interim Report #23 - Analysis of Sediment Samples Exygen Study No. : P0000760 FXriM 1'+'a+o<41 Nwabe .: roooo768 .o..b--d Mww .f Arl~r AiiA1.rnGL Mi7soD tww D~ivie .a( AcH ICA (lrOA) i. 9a1 y ell. f2! i.o w.aw!lq.~ld ~ 6.1 >f~eid1Y11ltr/~i~l~yaa l.1.1 /I~aa ~ OeQ ~eyriai d -lOD FrYiL d POA by w4 iy 10 wl at~id rd a llNesYl %r/ visl and6 I.I.i. 100 AL rrh Mr .l *I 7aL tDM laU a Lis Aavl~t.ddavr. .i .Yo .utrroArww .dlraYw.t io Mt. dft t00 wet. rIMiN o a irl vd 0f loiim wim.N !. a Ilf N[. IJa1. Ya1Ya P.13 A 1.0 pyai. IweB~oi~ ~oYtk . O[}!OA i rI1"w/ by kiqi.{ 10 aI.di410 FWeL MUM1N w a red w1im *11 so wMY rww . .111 .L [Lia .no .. 9.1A A Il1 pst&L hrINmWsrYiwo[?lOAYIArMryVwp;io MI.d Ru 1 .0 -OWLaYia N . t wLr .l'100 .i ..s.r i. .waLiD/EU.uY . -d 9.1] A 6A1 VIId 6Bfeda d.lYn d PpA iu d by ynrynj 1 6 AI. if b l IWsL "rd" to a!MI Tolre of lOD wi! . 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Patr76 of6S Exygen Research Page 67 of 110 p . 68 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 Exy{eo Pmtowl Number : P0000760 ell ^ swam 0800-6 r .~+M. .a V...Ixi ANALYTICAL 111ZTYOY Ndeldb.lYr.eri.Daws4wo oilubw9ewa.iw Ae4 (PFOA) i. Soi l by l.CM&ws 9] 3 A fa WM eld ae (maim NaNq XmMy.y MW mM arA 10 armed" 09".*L l3. . Mom at 00-eW allryis M.dr 6 i. l3aL p.yTnpylaw ow 1IYCbPC.,7lvhoswka !1A Aiw.wroMme r d oweMr .tlor dw m d. mW r-y be rqr.d r we" I00 1f"B r w )G.1 sub 68" of MI*lu AQ.iW (tYjiWY ]0 w IM) meal icYJ 9 r lea am, nr.d ewkY (Fioll .Wt a.Yq S sL nt wrhuol) and we xv a .awl R.tle.~l a brw ew ow raw. . 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MR ft tmMp.a .t Os b.Oi me and 44 to ad of . ..qb nt 0W.1 ro6wN ar be W~.~~rlblwrw~rySl~rooY A . M alY.AVwr o tinaw d t.rtJ+ PAVe 77 of 65 Exygen Research Page 68 of 110 p . 69 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 e=yra pmtw 1 N+rabw voooaf60 ' .wu>rmAL~ k.ro.. A. .4. . ,ra... k.`,a a OIS;$ l Acid rrray .sw s W 1t0 name arY*r . . .is ,q be a Ww+ . ft leoW.ri of . .. fiawNd W. ftwre wYwd r .rib ;nsyrd w~er 5-W Naw1u 1r sent r a .nr w dao.at vandrwi b wt w cwk e tnew w1 wo oimb =s be 6w Er rllr fejwih a L m mmqk rc 11w Um rnlri ewm hr emodsM" Urv xNabu1 eww w prYM b r adYY by 1'ewrwqiw = R Ux w*WiK ofOwt Ka 40MYN w Mftd SOWAwerfs Oft MrsL7aw 33 (a fpnWSkrl mRwaryww t=plr ww~ i.Y ~ swW w-d wd w wora wpf sn n4 Ow aewl vUwjwd wAww iYmid be hd r &Aud al r4 roynr . 1 3 A Mo'I~ MI ~M WAIN iMo a Pak of @ kyMut ion at SW ou Is. a yuna of 413 ML 1L 413 w D WO asr~etl to tlr Pr " maim wkik dw vWlr no (70 mi.) M ~ d kw daia r- id. 133 1iMlo1 MWir w1 sl eoaew MIOA d Web OwYr 6 a tM LOQ. If a MYt =MMi1!OA ~ 1rMb //~ 1W 70 tWl. IM a ~ pl~t rmpk wnM MaYWdmd ~M siM v.t mobs wa u aqq. 17 .3 R~eswiw of owl wikw ~d r~na ~4 rrt M Mv~ M13^ 6f am s... wlaw a, m~YOI qv1w eJY aw .e. W. .a.p.w a.rn. We .a rl uo%r. ..rwwwapl.wrN r .laabb,aw.- a~ Mb* ID Aq ..Wis a ..~ .aaa 8pk. aruar lo. if t i- Is 1 3.4 Aq aidnYn rrdd bMd is be a vlhtlnl wiGr by u Wft Oe lMqc Lwt 7ar, MW M aeWl 1? a dr eleWma of do ChWArioe own Newrr. dW ekl arYr i 6osr/ SAIMe aMlrb that ewb h tIW vYt W slow 70% of as MW IIIOOW of EMILUd WOEUOt w-.+. Ms '[L se~YUr amllkiwt w !r n11W6 m ervr po.rrl ..0 Si. w+tn pc' =sa> if e. & .b.. ~..w hr aro k aim o.ra am I 0W M" ON M rtr ID 800 WIII~IOI 0/1[RiMS w 6e somd" vlr wlwm t an atunoL +edd be welya l 13.6 land= Ihs Mr M aMti o/ wmql e wl on OR nas W d4 % .hlia s aYytlal ia $ ewrr m ar wo.M ibis Mob .u4. s aqp W sa un r w . w rm wyse. r.r s e, Aap 29 of 6s Exygen Research Page 69 of 110 p . 70 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 F=yyrn Protocol Numb. er. P0000160 s.a.R . .rb Atrhed .lAryi. wrirl;.. . wa+u AMAI.l'l'[CAL 1MiT8O7 l .D.rdn i.idMkrmemric Acid (i0A)uSoil r LClDL1IH8 14.0 pMLduo M.1 0020-4rdy epris a wkrWe ie MwAk1 otr/OA brd (MWL. 1Mi ~ lrk r 4 uns 60 rOiw ww Oisv ni+Miu+ wu+asy) ~.rr b V .ltrr ys ..es.~n'mis: PPM M " (wL)- Q..t . w. . :. g ..n x or DP - how by wiid. Mw Arl wYr to.. dlrN, it .serry. 14.2 h soon ArdAtl Ms Im~ rwq o( PFOA pia to wttKiia. we 11r OOwy ~re~ y..!`Yr m. pww noovay. 1 -my (%) ' [ww ah*- orla - -a. bwd o "Dow (WO ao ..nR.maoWL) ~- 14J U- 14 ib+i% . .to.. to Qaw1t i6~ EMM u( "OA bond is nj/l to awL(>kf RoAll..e(wD)' ftt+a_a~t..a.i~ .~. am~~ma~l ~wNw~u~ 1 4A Uw do h1w.ia e g&Wm 4 eYaAft Me a+wst of PFOA fwd in ryb Yri a!q fwW !!OA fmar (pA) dry we;* - TlOA 4 . e (pp3) : Itoo%r towl l oli4flcll hy. 7 .r+ Pbpe 2Dof6S Exygen Research Page 70 of 110 p . 71 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 8cne4 Protocol Nurlbec Po000760 ANALYTICAL IGITHOO lYiad tJambw V00017p Mob" of AM$MW hr at WlnfYrYn of Fwaswese"aw Am (MA) J2 99"Mu 16y LCAMl6 . HpwRw~ pMuheal7LtiyPsr S 3m ROMWA Orin i1WG1OOk PA1p01 APPOwfl~ ' b~ CMD rRYdwl UNK.LOMIL ROOM Az/ cof~ela! Dw - TqY)yr: + ~' Poge 30 oJ 61 Exygen Research Page 71 of 110 p . 72 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 i-- 5xypea Rorooot iJumbu : roou0760 iq~~~r111N 1 bow IM/. Vogl yJ Atu1LYS1CAL ~S710D MrblefAUlyjbbrdr nqoi~dr. _ _~ I.CJIIHiM! . ~ . ~ . :, _ .--.M by 1.0 faP 7ha rlw~ ~ r h~ryM 6e ~O lelia rd N~ of ~8oo~cunwc add by 81M WO parx tiwid CYoMO/qY oawrr to a rroew man 9p .cees~~~cDWarr (Lf'Ad911~ i~ w~iro~ . zo arb Z I A WW OINw Mh MaWOl7 W tie s 21 CwaY 662PPnpar4M LdYsrlins sq Gb--=-_ k faaw vn~wra army )A lqM~qo~~t 7.l AtiwtN~~fMM>yN>tr~ea 3.2 Wwr4ow~rA~randUMNOrr[Nnpa].3 Jlompiw 11qM ~Ef~OO rwLL !b aYOwad to puilibw r roam oo~rwa AI Asor~w .~rari~wwr:.aebsMia{wolas .rnanro~ sJ 11 ~/1. m1Lr:m pccW rw .iU bM WwqrW a a ..liq .Mn h, ,h . oi M a0 Nwm ad L .eur {.1 M4rr- HK.C V@& 4 2 wwww-1a1 .CVe. u As.uoAs;a-1.q.cr.& 4.4 Awrr Ao W r- A.CA . JlaOrt 0" 0 PINAAWSOCOMW AdO-Sip Alridk SA ireoa w aw l4 Vors 11 A 1lo }rYa~w keY *--910 -F" of 46 2 wbrw o'PYie 1 oft o weWlo voles Yyamr nphA of i oaMS 72e0 rLwrwaod M o1d m Mw Nps 6m Mr(LCA1fM51. Si AloMarwWa ww dft bpk oepimod pmrr ~ 7J Adyurdlabum vr" dwoft ra000D1 & SA $0 . L +" .lwrbrd"kw w&W + bw Si ts ac lIr foww ~papl ooda~ r. .. s.i 01~r1Ydw~i~OrUP1o0wL 100-2GOd.j S.i13f-rL IDPE ns w4esft bwOr. $.t s Ml.chrlDltriJbt s.+ DYVort.roror. f,lo Ary[p lWia (MO.N00 Yf. me 10700 MW. sk3 dwwili* +yr. 5.11 aws 59 ht Vn 6 c1V ICI VI wtMOea 5.12 D1R ~ orAIL r. ..~r+ Pap aj ofas Exygen Research Page 72 of 110 p . 73 Interim Report #23 - Analysis of Sediment Samples Exygcn Study No . : P000076 0 exyieo RvmoW rn MW - rooomeo w.~ .. .+ ~.. ...~.~.~w A"YrrcA[.eSTew u.ed d . DO ...rr . .te~k (PPOA) Ms.&~. ~ Lcjha&ls s.u V . 5.14 W,it-.a.drr.. 711 Owrlt Pg b *hpi m e6 SO O1. MlyAyr *- oi r 3000 q e 6A GLaYy~Yie~7r~ 6. 1 /1 wWYY CaYwal 9 Yr tr (Jf~pre~ Se~yite), 2.1 eu~ i SO taa~, f y . QMt: Wvs,= )70) [2 Tmqarwe 3PC 6.3 06UUArW : 3WA~M~Aauuillo 6.4 Ma Wb wr.p) : wir.a 6! GMir 1re rs r, Itacfaal IA OA 63 63 ~o a IoA ts 11S is rw. Rare ri B lalaa.i 33 63 3s 6.3 7s ~.~ ts a .l 10 0 .3 6J 66 ij~~V~Y~c Ut1.kY6mrr6lrurw~hu70MLl 6.7 QdrYsc R.tAiu-arrl .ruNWOndoaw~.w 1.7Lc ~]7 . :r. ?Mr1 OwNd~r~n iir6/6 u a P~ d r710cwn01d 'm m~Yr a a/r~ r Ie LC qn a 9.0 YiAdsbr r 7-1 ~ ~7ArNiptlwia3[ad~~miree~a3rl6i!s~zbr TM AM w6Mer M rWrd r 9 Oft ad aay l . * . .V6 i. adr a n+. . # . WM r.. . to requ dla4fm U.S NoAik Rw ~.~ .1 1 Yl[ ~ i~lw Y rr1l r D~'~~6 aJ ~C6w6 a u1 j n( Mewiirw.r to IM .i .l.r.- bp7 a . Page 32 of 65 Exygcn Research Page 73 of 110 p . 74 Interim Report #23 - Analysis of Sediment Samples Exygcn Study No . : POOO0760 Bxysea Pra0col Number. P0000760 sfr~a WSW >r.r. vori in D Af1k1.N11CA1. MM/M Ix ai . "Kas>.swl xreul qwwAw* AM (TIOA) bnlriire.e by LOU"" i2 )Dttwms N)trloa~ i21 :x awi r w ia wlr r'a, rod by a0"0 10 d. a/ acwk aoo a lOrom[. .t.r.. 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Cap. vYn at aSdn w a vinl ew dk J. -30 a:a 11.7 C.rdrr.f .rf .rJeB6,P.f.r -2oarr. 1 1. 1 4~wtOet~NwoarrRla~Wr, tblfuOaNwu . 3Lf Wall 6M aoIws .BY 4 mL derd,d CdlS 1M aLra oW add 4 A d aLm1~rt%arp I Ia. I 1 .10 (1NWWau1eB0CNJBtoYi1/(1 c6OL)Yy posing I6 Ul .a wrnol 2 IYwB ly 20 >tf. M@LC aa w ( - 2 bop4wl. Ao r MM aolow xra Arr 11 .11 Add.S rOrN Y+260 m1. N ~ ad bN ea pN jsae1 ce - ner.d BrE ewid w IL 12 YY v1% -4 m6 10071 n pma. Collect S sL o f duW~n in WWuHad u Lr4}qJd ~r1+Grr wruft - s ml) I 1. 13 Arlpra.ep lr .iy Wa opq LC+MB4 6. rw1er? PcgeJlofOJ Exygcn Research Page 75 of 110 p . 76 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P000076 0 fxyM Protocol Number. P0000760 ~~ ef DWI~ ~r~b lf~I/AYr v010171: -771 AKAi.Yi7CY.la'I46D M Dwifirus ' Add (!!DA) i~ SdiW at by I.GIUII 0 12C O== rfvOq 111 1 oM M rwomwMef we d6 +rV1~ ~d >wiRd rqyi ip t1e 11790/M/ qMoa A uilMtioa StanAM wwq ~ncd~ W felbr pit ~7ed 80"i - It3 l nOr* OtlOA.aW s ev"ooft r 49 L .MMvwonmae Vrieale-J$ r r :riw . eN re f2.7 AMM rb wi Of swwld aYlmhr ~dri am Y isWd W ON e**Y4 r r M ad d rllYm NL.7 7- 10 MI19111 a m Al N 1. Nc ll06 ws YraMY9y . nMt tlw he t i-rrnwa in S of GIIDUtm OAhpb my 1s Wwrr a MrW61 t Wq. M6 w.ry a. Mrfing 5 . 10 mow ot . (b .r Glb.d oor b! y s+wrno . Moved 0" f i .iorr aw, ed Lwle. ...a .ai .u0 M b. ,.a wl iwjrti. . .r"r a 17.6 Wperr1N 6 Whralm 4*ftpi w- by MRWr Vwselwi-"prr1Y1tM]dr rWvi ipredidaoptvpwwtaewe rwir nY1lYw wIMM , I n aWrd ar,wurwft viy MrLy= 72 ppr .qri sOkrl lIS !OWW n WM dw.Y is -wd oYwd rw9sR ANY lreoles tlrt su! Mrdd qr. d.dA be lmYar k1t+d ad n"yMd. 1~ .a A. p4w- O ftle 13,1 Jq 02 173 dw "Yere ruo !ow . pie 01 16 AwDOer i " Y 369 .sr finn - pwa ~. Y1~ 1l l~M r~et mwpe~M le 1~o TfOA aiiu~, whik ib dsylir iM (W ."a) IrwM~ W low oEe.bc . dimide. MAW bl eb Mask aoniW MW NM COrITOA s hash PPOA M MW P~ OM 0.2 V Mw Bw Ua yid.. mw 1h LOq- Ni en. Olrnt repY aor Y ebMW rdlrron Nt em M ias-c+d. tw ..ai. Of aol *Ys .i =OS Rm. mw to ewww 70-130%0( IYi lorw Vat. a . .enol 4pik . +1t1 . ea .a. Is ucAeeM i W. de . fir fia ( aN pla AcuL 1e noostid. Any n~r'v .pik. -bid* 7P aft SWJI M .nMa`d by 60 mob" a 6er*ioc it rxaMtian .4 wWal"d 17A Aqr dIY9Y ft wedwb !wA b I. a " Ytf W W01w by wAt& Jr NuOe 1na 7>R ~q w MW Doo 4 wlwlrNa d ft atlbctlae wne . Newnt. die W r.M d wasohi WDnt " Na/rM IYr awiW Or # YY6A sot is uerE bri of Iy m1 wNr of mamma WdrN 13,5 Mrw.va" .rYM's OOdlehl (R) f0[ oY4%H00 - p-wd am !s iA .992 ~ 7JY.9gS) it qlllOM INYIY ill OIiO09 iYl ilAp . 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AiqmW fiver - 10 r1M~M ' Pope S7ofdJ Exygen Research Page 98 of 110 P . 99 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 ^ E~c~omPcoti~oolrFanbsr. Pouuo760 L~L~r YbM/iie VMpl~f - AHALY[1CA1. MC170D Arl~ir~ iri~ h~'~wcid )k~wati MM" Iww by LCIMlIAQ 34.2 Fag W6 rWi Lrw ~ of rWA pea is . Ib b~w+y ~P~W b OYmIM M M'aM+.w.~7. eweda, wr RNCwfp(~' . [ m . .u,b r..~awr.i) ...a re .eila .c.uw (.MyaJ , lor ' aybdd~+prda i7 u..rbM'i~{rpe+ba.r.~w.,aeuuorPFOArw .rmw~+~~^ rsbr~~ rrws Mw or~- ~~tp lW ld t Page Sd of 65 Exygen Research Page 99 of ] 10 p . 100 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 Exyjea Prolvvvl NumDnr P0000760 AWA:.Y'nCAL METHOD Wrvarreeie VOW?" M1601 d Aa .bA br F- pMwaYdr d hlws.uwwk AMRPOA 1 ~ is.. M. ...ia.. .yLCataw AsVy6wUssAdiT lryM trM U wst a.mrcb anw 7aa Cotkvx~ tA 160 01 Apq+eoW By. PW CQmft Dr~ 'AoLied Lr4. LG~ 8 "M 1"w h S~.oAuLffL `4>zr . lYir / Vio~ IT+~Y Orw is. hYom l~el 7" Tya t, Pw 390f6J Exygcn Research Page 100 of 110 p . 101 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 e-1 Ox YLw rM oo01Th>mbr:P00D0960 lkw. 9afm. Ndl9~ WOO17M AMAI AL Mrva- Rl.r = Of ft u .WN6" w r rrs~ AeiO (rFOA) 'u $wII 1tWWW !wo y 1.CJ9tSA!! 1 .0 SO " Ytw meow is m b. 11vr1 far tti iwlada O i pv~iura d pr0aoaseuewc ati4 >P ii* ffs~saaaa Liquid Ckwo -OlopapY avP~ad r a WVem Mw Sawwarit DwsM gOm p) is now Msaal anr 2.0 iaMy 2.1 22 ~>Y. ~,Opfe, xv061 .as l.ii.j asy e7u.ro1 rw 0~wumy 10 t wpl. Lp:,wl - - 3.1 AcIrlL stud .wb baawaq 7 .2 w aa~~li pw~ia~ Y awi6 ir aan~ awoi.. Fbw..ar . 11aao .wwn .ww ... q .llw96ra0~pl~rld+rr iae.ls~p. .u~. UBa. v.. 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A1ro~t~ re6a. sl M~prad. , r~n 1 ~r Pbgs 61 oJ63 Exygen Research Page 102 of 11 Q p . 103 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P000076 0 10- Exxon Protocol Nutmber: lOOOD760 7aqa laia.i Wa1 NSIOr vro01 M A}IALTilCAL OMiT110D We *Ad atAaal>.r br 1Aa D iYitaaaaa aiaawaw a a aa ..w c-+1 i =S-a L-9 ioo rid Soon y LCA15(1[S !.~ 3na1d ~.rlw f.l ~ea~rt frdll~.il.uaaMMtaa mok ~olaCan oI-100 qI.L of 1POA y vt+ahu4 I D q Of ~YNed>~dM~ (aq.~a! ~ iMltY) a716W b 100 0l. rwlr iol's a 11s .w1.1De Oarla. 9.1 .2 A 1 .1 iYuL h4MfMia wkieoM Of TFOA is AqanO by Mayinl I ~L dtM 1 g0. PO'aL mu air N a iW velea of too vih .m..a in S .129 ml. LOP! book 0.13 Astw WL 6WANAN a+riratrFOA'rwer " be.:yi " 1 0 .I. 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Arty waP1a W amid Y.eaca ..roor I6wiu be Whir 4Ata1 aal ivaaalya. L hod W ' Page 63 oj65 Exygen Research Page 104 of 110 p . 105 Interim Report #23 - Analysis of Sediment Samples Exygen Study No. : P0000760 Sxyjeo Praoaol Number: F0000760 . . w.~~ r . . .+~r. wwn. ~ u~w x-ncu. >a,c>two o ,aw%Ori~ m~i n ~~ Acia MFOA) - - - w~rs .rw r u+Idt~Ms . , 13A Ar FWA C1MrL 13.1 Onnawrr eaM sliav a Pak ef ArOlr iM A I 369 an !r, a perw . . d413 Oft This 413 0e 11 Pwr 40ew41110 00 FFOw 11aioq wWs ft - e~/" 1q(7a~OnM~~rtVle~d~WN o ciN 13] . Ni~ 11i~ ~1 rt iss Iib "DA it levels rrsr done she lAQ if l~li onro~ R~A K MMr Poisons Om 10 af od . 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It wlirrios, na b AU MWOAe Ww iGw, 'Is +i " Y shops m a be YYa in Wpm iwvo rt eya[iw. -a ft srWEi u N . nUn t r dwiM MW be ewlyiW. 134 3rwn don Yr..r ardri rM woqtw a sri ow *d some ane, : 4 x .s: .rr3mrn. r,n ..a .ci.oaiit .rcaJi .naa . ;~h~o as elylirl as Ye 69 ow moves be essailyost Ia0 CYaY oWu 14.1 Ua~fl~ .to0od~~Yl~b~ala~4~ moo" ofFPpAfaMd(w *mt. rd o F ook spa) nag b scald vim (li swr tMtwdon poratwow Nws- 0 by am M M L) a sMn pow- F0A Ard bmAo l) - M dc s . iej eocr) : OF i Amoisce base slope Df - by Mtrir iYW wWae was mWd, dmarrx N4 .x Aaa- 30 w rCf "MI/is, be"" Oi+ bCIY~ MOsOf of /FDA PYC! 0 O U ItC Lm. v[ v know" oNr+. n omru aw Foneso -.r. a...r(x~- ~ .wt.s .i~~ ar>, .aw : ... ..iiwid~t.)) ,im .w>~ .rw(e.~w rw . ~ PW 64 qf6f Exygen Research Page l05 of 1] 0 p . 106 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 .-~ Cuyacc Prdoco] Nwnber: VOOW760 ApwLYf1CAL MR9OD dArl~ tbDrw~iir Aaa AI~ MM LM w s.,an by c.OSpM s 14J UM b 61wiIK etrG m lo eawt 6Y smomt A! rFG \ fws0 PA. wyid. b 1Yf)A /owl ~ppb) ~ +'+" ~od f~~t 11 ln~ wlad r~~ u ~ wqM ~Mvr ia~l.) 10~ .r~ . W)~1' Page 65 of 61 Exygen Research Page 106 of 110 p . 107 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 RESEARCFf 305a Ressaah Orin Phone : 814-In-1039 State Cotle4e, PA 16901 Fix : s14231-15t0 MQTOOOL AAAENOMEMT Mnendrt W Mimber_L_ Effew" DOW 011190 E rygen Sh* Numb.r...P W= chat study Nui, t er. pa .1c1 OED CON 1) And" Procedure Strrrrnry V0001780:SeeUOn 9.1 2) venTiabon or Aiwyecal Pioos&,ro t~e /1MUDED T O 1) Add b Seclbn Y.7 : Sectlon g .1 .0, Akemeq wefpNh d alandande mey be ueeC to PhP M mkwr aM oonantrarons of sbdc eduft e n rrosseery. Apemees Isvsls at brtNnuon nut= n ~ d a.p.ral. Low wW No sokkV2) an.tylee for ach nvtrb i may be alWna dependn0 on sa~rpis she WA YWe Ibr **action and/o to cover snayte aoncerttratwns e)Vected I n tM arnplee . 1) HWW ~~ Of ~~ In oader to spice the umpla 2) The snpN ohs a Qh bie for MW maltrntl 1Yrr end anrm wp inhaler fm ` .% eoq~~d . SaRdnp at UN prsdshmrned lewb In to proloool Pus ft spiced oonanaation bwrr tAen the ftbCj on pelt Ne.01M uWyN W4Ne in tAe 9rasid Wider uncles we w9p kd b WMtry eemeed the P+sdMermined apUg i+AN Asted In the Proloool. VUhNf ifie kviels h 11~e atmpbs groetbr eooond the apid~~g Ir~le . en eocursls nawwy wk* cemot be abulaoed for the QC it . higher spikkp levels it tM bathes WO or fhe anadyte oonmnbatlons e3p ee4d in rie +wler somplee . OThAe LiOmQfLs1^00~hr e Q 1 C selrfritp~ ls d ~ g~D?Y smaM mmnal Ow and is 1000 %&L for a sample oi anNl nwmMl nnim. Hghor ~ co epYci~p for tie water amp," wiq enwe that more GC reaavery dala ~ wr+ can MOP ~ 1 7 A aS Eiryqen 41W fiavtew ~,,'~S at.le!. ~R' tJ9RIiRY ID YVOO0t22Ei= _ AD1uwSfliATivE FOR M Exygen Research Page 107 of 110 p . 108 Interim Report #23 - Analysis of Sediment Samples Exygen Study No . : P0000760 RESfARC H 3038 Research DrMe Phone : E14-272-1039 Stnte Colllql. PA 16b0/ Fw 314-231-15s0 Anvmxlmsnt Number Effeetlw Date: Exygen Study Numbar PROTOCOL AMENDMEN T 2 03107105 P0001131 fXiant Study N+:mber. Peoe I a 1 Nona Qgg=T N 1) Report p%* 1 f of eS 2) Test Mlaietials, pop B a! W. PF08 bant4lon matNdsd 49g ,s 99. B1~ 7~ 1} In~Oend d ons tkrl ~pWl, Inl~rlm ypoflt WI bn ita~d . 2) PFQS tansllbn monitored may also be 49D,> ee . 1) Due b the szOeNivo Wass of to We Mb,lnOeft repa{s wit be isetwd to al>ow the dwM b ntoeirs date In a NmAwoww Pm+nco- oyLdr 4as 2) The AS 4000 LGIdIf,iS syftm dfttt ft 499 .a 90 PFi03 trandflon with gmater wtllMty IM ft 499 -> go "Now, IMPACT ON ST~JDY 1) The alent wiM be " 10 Mcalur and Wow the diThown qufolc~r. 2) The 499 .a 80 U w Ntlon an be detected with greater seiaitlvpy: tomfbre, giving E bel9e ahompDqrapfry. 9k~y DOW AA- Obeft" 0 o~+~ l~ evor.e s~,q h~.a~rn cr. .b HOr Dow Exypn G14u RovNw LewRY ro: vMMa - :: Anurwe*PAnYE FMM Exygen Rescareh Pagc 108 of 110 p . 109 Interim Report #23 - Analysis of Sediment Samples Exygen Study No .: P0000760 ~ ~e 3058 Research Drive Phone : 814-2721039 State College, PA 16801 Fax : 814-231-1580 RESEARC H DEVIATION FORM Pao ,az Project Specific Deviation _ Facility oavietlon owe of Occtrrence: 04116/06 Exypen Project X : P7EOIP1131 Deviation 5 Client Projed if : NA Reference M : 06-076 Regulatory Qdnc Deviation Tvoa : jlnct* YM krrt efhoW and SOPa) GlAP X ketDow X GLP Other vw NA None Notebook referenw. NA Samde t>.scrleflon Method SOP Login d : i.0006191 CorRainer # : NA Lot d : NA Sunuearv of Oevtat[Dn: The three sediment samples in L8191(CO172892 - C0172894) were orfpinaNy extracted using the aedinront method 110001782 . Poor recoveries were obtained for PF08 . PFOA and uC PFOA . Because of thb, the s0udy sponsor requested the use of an alternative eXtYlaCtiOn for these compax+ds, as foioMra: Dirocf Injection Method ; Before th e samples were weighed for the extraction, they were mixed thoroughly by vigorously chakkp the container. A oneyram portion of sediment was wooed into a t5miliMsr centrAupe krbe for the extraction. Ten miAilliters of 196 acetit acid In methanol was added to each sempb. The samples were then shaken by hand, valexed, and sonicated for thfrty mhwtes. The samples were then centri7uged for - 10 minutes at 3000 rpm. Each sample was analyzed by LCIMSMAS eleclroaprey. Using this method acceptable data was obtainsdfw PFOS. but the neoveriea for PFOA and '3C PFOA were 301 poor. Another apemaeve me8iod was then used for PFOA and t3C PFOA, as fotaows: Af ftmailve SPE Method: TTrs samples that were We perad in 196 acetic add for the direct injecflon method were used for ttrc exliadion . FiMe miYiters of each sample was diquoled Into a 50-rnL polypropytene CsntrlhQe diDe and the vofunN was taken In 40 mL with water . The samples were than cantriiued for -10 minutes at -3000 rpm. The wperratprM was then Waded onto a C,1 SPE cartidge conditioned with 10 ml of inetlwiol and 5.mL of water. The eluab was d'acardod. Approximately five mlliuters of methanol was added to the cartridge. Frve mtaNMters of eluate was collected Into a graduated 15 mL polypropylwia centrifuge tube. Each sample was analyzed by I-C/MSIMS eloarosprey. Cause : Preparation _ Analysis Instrument Client Request X Other knuact: More usable data was obtained. LIBRARY ID: V000t840$ ADAMNI-STRATIVE FORM hxygCn Research Page 1Uy of 11U p . 110 Interim Report #23 - Analysis of Sediment Samples Exygcn Study No . : P0000760 E) . T CHEH EHSR 236 1B 651 T33 1958 05101 '06 13 :46 110 .106 03/03 ..6f-91-tON 41 ,blp Fro*-IFM3q .Uf1ORi + t-04 FAUN) P-111 .. . . ' . ~, . . .o . , . ' r . ~tl . . - i. . . Mg RtKK N~ ~V1 0~~ rl7~elw. .IT kAa Cdfqs~ M 4H~'1 8'1}' 1J 6 ~tTK31Y f~iil~i;, , r'~`~,`.; , ;, `' ' , ' .. . ' ' . T ~ .T ; ~~ rt~~~ ~~~ ,~ , saiim "*Milo : .UMW , ., ~ .i y~ . .. , '. Ol4(pM ~.. :, . . ,~ ._~. . . CIRit~M : .,,,~. ..`r " 111~~w~ : r~~- . . ; -' .. ' . .- . K "- i . .~ ai ^S A .. . ,' ' ' `~`;~?~' , " s ~ \ . .Y' r ~. . _ ~ ~wMAwuAnW _ k . .. ..~ . . - ,', ~ % , ' . . ' `~;::.: :~ . . ~ . . . .. 'Y`,,''Mt`'\'I`I T . `' . ` . r '~ J . . . .. .~' -' :.t .(rr?~{}~ . . .\+ ` ~ . ,. : . ~Y ~.w .h , .. ' .~' . ~ . r f, i .: . _ ~' ~~, tr~^N y . . ~. . ~ . ~' ~ . . . + ' :. : _ 'a~,~'M~~ ~L'/~"~, . . . t '1 , r . `. rs . w :r ~ "i, . ` ? ,ri . ~: r . t.^ . - ' , " ; . . .f ) ,'~: , ~ . . . ` ;: . . ". ~~\ ',5 . , M , ' , ' ' . , ' . . . M ~l .M . . ~+. ~' .. . , .. , . :)f'r ''S ' '~ ~'~")' '~ . . : , ..~ .. A,.' ; . , . . . iNO l IV. .WYud" . , . . .' ' ' , . ' ~ .\ . . . , " . . Exygen Research Page 110 of 110